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Sample records for efficient one-pot synthesis

  1. An efficient one-pot four-segment condensation method for protein chemical synthesis.

    PubMed

    Tang, Shan; Si, Yan-Yan; Wang, Zhi-Peng; Mei, Kun-Rong; Chen, Xin; Cheng, Jing-Yuan; Zheng, Ji-Shen; Liu, Lei

    2015-05-01

    Successive peptide ligation using a one-pot method can improve the efficiency of protein chemical synthesis. Although one-pot three-segment ligation has enjoyed widespread application, a robust method for one-pot four-segment ligation had to date remained undeveloped. Herein we report a new one-pot multisegment peptide ligation method that can be used to condense up to four segments with operational simplicity and high efficiency. Its practicality is demonstrated by the one-pot four-segment synthesis of a plant protein, crambin, and a human chemokine, hCCL21.

  2. Efficient one-pot synthesis of tigogenin saponins and their antitumor activities.

    PubMed

    Gu, Guofeng; An, Lian; Fang, Min; Guo, Zhongwu

    2014-01-13

    An efficient synthesis of naturally occurring tigogenin triglycoside 1a and its three derivatives 1b-d bearing different carbohydrate moieties, as well as their antitumor activities, is described. Partially protected thiogalactosides bearing unprotected 2,4-OH or 4-OH groups were used to facilitate regioselective reactions for one-pot sequential multi-step glycosylation, which has significantly simplified the target molecule synthesis. The synthetic saponins 1a-d exhibited much higher anti-tumor activities than the positive control cisplatin against the human epithelial cervical cancer cell (HeLa) as evaluated by CCK-8 assay.

  3. An Efficient Protection-Free One-Pot Chemical Synthesis of Modified Nucleoside-5'-Triphosphates.

    PubMed

    Shanmugasundaram, Muthian; Senthilvelan, Annamalai; Xiao, Zejun; Kore, Anilkumar R

    2016-07-01

    A simple, reliable, and an efficient "one-pot, three step" chemical method for the synthesis of modified nucleoside triphosphates such as 5-methylcytidine-5'-triphosphate (5-MeCTP), pseudouridine-5'-triphosphate (pseudoUTP) and N(1)-methylpseudouridine-5'-triphosphate (N(1)-methylpseudoUTP) starting from the corresponding nucleoside is described. The overall reaction involves the monophosphorylation of nucleoside, followed by the reaction with pyrophosphate and subsequent hydrolysis of the cyclic intermediate to furnish the corresponding NTP in moderate yields with high purity (>99.5%).

  4. Facile and efficient one-pot synthesis of benzimidazoles using lanthanum chloride

    PubMed Central

    2013-01-01

    Background We report the synthesis of benzimidazoles using lanthanum chloride as an efficient catalyst. One-pot synthesis of 2-substituted benzimidazole derivatives from o-phenylenediamine and a variety of aldehydes were developed under mild reaction conditions. Results We have examined the effect of different solvents using the same reaction conditions. The yield of the product varied with the nature of the solvents, and better conversion and easy isolation of products were found with acetonitrile. In a similar manner, the reaction with o-phenylenediamine and 3,4,5-trimethoxybenzaldehyde was carried out without any solvents. The observation shows that the reaction was not brought into completion, even after starting for a period of 9 h, and the reaction mixture showed a number of spots in thin-layer chromatography. Conclusions In conclusion, lanthanum chloride has been employed as a novel and efficient catalyst for the synthesis of benzimidazoles in good yields from o-phenylenediamine and a wide variety of aldehydes. All of the reactions were carried out in the presence of lanthanum chloride (10 mol%) in acetonitrile at room temperature. PMID:23919542

  5. An Efficient, Microwave-Assisted, One-Pot Synthesis of Indoles Under Sonogashira Conditions

    PubMed Central

    Chen, Yu; Markina, Nataliya A.; Larock, Richard C.

    2009-01-01

    A microwave-assisted, one-pot, three-component coupling reaction for the synthesis of indoles has been developed. The reaction is carried out in two steps under standard Sonogashira coupling conditions from an N-substituted/N,N-disubstituted 2-iodoaniline and a terminal alkyne, followed by the addition of acetonitrile and an aryl iodide. A variety of polysubstituted indoles have been prepared in moderate to excellent yields using the present method. PMID:20160894

  6. Ir-Cu nanoframes: one-pot synthesis and efficient electrocatalysts for oxygen evolution reaction.

    PubMed

    Pei, Jiajing; Mao, Junjie; Liang, Xin; Chen, Chen; Peng, Qing; Wang, Dingsheng; Li, Yadong

    2016-03-01

    Herein, we achieved successful synthesis of uniform Ir-Cu nanoframes with highly open structures by a facile one-pot strategy. The key to obtain alloy nanoframes was the careful control over the reduction and galvanic replacement reactions between different metals. The as-prepared Ir-Cu was proved to be an effective template for constructing trimetallic nanoframes. Furthermore, these highly open nanostructures exhibited excellent electrocatalytic performance toward oxygen evolution reaction in alkaline media. PMID:26864283

  7. Highly efficient one-pot three-component synthesis of naphthopyran derivatives in water catalyzed by hydroxyapatite

    EPA Science Inventory

    An expeditious and efficient protocol for the synthesis of naphthopyrans has been developed that proceeds via one-pot three-component sequential reaction in water catalyzed by hydroxyapatite or sodium-modified-hydroxyapatite. The title compounds have been obtained in high yield a...

  8. Efficient One-Pot Synthesis of Colloidal Zirconium Oxide Nanoparticles for High-Refractive-Index Nanocomposites.

    PubMed

    Liu, Chao; Hajagos, Tibor Jacob; Chen, Dustin; Chen, Yi; Kishpaugh, David; Pei, Qibing

    2016-02-01

    Zirconium oxide nanoparticles are promising candidates for optical engineering, photocatalysis, and high-κ dielectrics. However, reported synthetic methods for the colloidal zirconium oxide nanoparticles use unstable alkoxide precursors and have various other drawbacks, limiting their wide application. Here, we report a facile one-pot method for the synthesis of colloidally stable zirconium oxide nanoparticles. Using a simple solution of zirconium trifluoroacetate in oleylamine, highly stable zirconium oxide nanoparticles have been synthesized with high yield, following a proposed amidization-assisted sol-gel mechanism. The nanoparticles can be readily dispersed in nonpolar solvents, forming a long-term stable transparent solution, which can be further used to fabricate high-refractive-index nanocomposites in both monolith and thin-film forms. In addition, the same method has also been extended to the synthesis of titanium oxide nanoparticles, demonstrating its general applicability to all group IVB metal oxide nanoparticles. PMID:26824518

  9. Efficient One-Pot Synthesis of Colloidal Zirconium Oxide Nanoparticles for High-Refractive-Index Nanocomposites.

    PubMed

    Liu, Chao; Hajagos, Tibor Jacob; Chen, Dustin; Chen, Yi; Kishpaugh, David; Pei, Qibing

    2016-02-01

    Zirconium oxide nanoparticles are promising candidates for optical engineering, photocatalysis, and high-κ dielectrics. However, reported synthetic methods for the colloidal zirconium oxide nanoparticles use unstable alkoxide precursors and have various other drawbacks, limiting their wide application. Here, we report a facile one-pot method for the synthesis of colloidally stable zirconium oxide nanoparticles. Using a simple solution of zirconium trifluoroacetate in oleylamine, highly stable zirconium oxide nanoparticles have been synthesized with high yield, following a proposed amidization-assisted sol-gel mechanism. The nanoparticles can be readily dispersed in nonpolar solvents, forming a long-term stable transparent solution, which can be further used to fabricate high-refractive-index nanocomposites in both monolith and thin-film forms. In addition, the same method has also been extended to the synthesis of titanium oxide nanoparticles, demonstrating its general applicability to all group IVB metal oxide nanoparticles.

  10. Solvent-Free Green and Efficient One-Pot Synthesis of Dihydropyrano[3,2-c]chromene Derivatives

    PubMed Central

    Jain, Shubha; Rajguru, Deepika; Keshwal, Balwant S.; Acharya, Aman D.

    2013-01-01

    A rapid, clean, and highly efficient method for synthesis of dihydropyrano[3,2-c]chromene derivatives by one-pot, three-component condensation of aromatic aldehydes, malononitrile, and 4-hydroxycoumarin using DABCO as catalyst in solvent-free neat conditions is described. The present method has the advantages of mild reaction conditions, short reaction times, easy isolation of products, and excellent yields. PMID:24282643

  11. Efficient one-pot synthesis of 5-perfluoroalkylpyrazoles by cyclization of hydrazone dianions.

    PubMed

    Ngo, Thang Ngoc; Ejaz, Syeda Abida; Hung, Tran Quang; Dang, Tuan Thanh; Iqbal, Jamshed; Lecka, Joanna; Sévigny, Jean; Langer, Peter

    2015-08-14

    A highly selective and efficient method for the synthesis of 5-trifluoromethylated and 5-perfluoroalkylated pyrazoles has been developed which relies on the cyclization of hydrazine dianions with ethyl perfluorocarboxylates. The pyrazoles prepared were evaluated as potential inhibitors of alkaline phosphatases, namely human tissue non-specific alkaline phosphatase (h-TNAP) and tissue specific intestinal alkaline phosphatase (IAP). Most pyrazole derivatives inhibited h-IAP more markedly than h-TNAP and had minor effects on nucleotide pyrophosphatase/phosphodiesterases. Therefore, the compounds appear as potential selective inhibitors of h-IAP.

  12. One pot, rapid and efficient synthesis of water dispersible gold nanoparticles using alpha-amino acids.

    PubMed

    Wangoo, Nishima; Kaur, Sarabjit; Bajaj, Manish; Jain, D V S; Sharma, Rohit K

    2014-10-31

    A detailed study on the synthesis of spherical and monodispersed gold nanoparticles (AuNPs) using all of the 20 naturally occurring α-amino acids has been reported. The synthesized nanoparticles have been further characterized using various techniques such as absorbance spectroscopy, transmission electron microscopy, dynamic light scattering and nuclear magnetic resonance. Size control of the nanoparticles has been achieved by varying the ratio of the gold ion to the amino acid. These monodispersed water soluble AuNPs synthesized using non-toxic, naturally occurring α-amino acids as reducing and capping/stabilizing agents serve as a remarkable example of green chemistry.

  13. One pot, rapid and efficient synthesis of water dispersible gold nanoparticles using alpha-amino acids

    NASA Astrophysics Data System (ADS)

    Wangoo, Nishima; Kaur, Sarabjit; Bajaj, Manish; Jain, D. V. S.; Sharma, Rohit K.

    2014-10-01

    A detailed study on the synthesis of spherical and monodispersed gold nanoparticles (AuNPs) using all of the 20 naturally occurring α-amino acids has been reported. The synthesized nanoparticles have been further characterized using various techniques such as absorbance spectroscopy, transmission electron microscopy, dynamic light scattering and nuclear magnetic resonance. Size control of the nanoparticles has been achieved by varying the ratio of the gold ion to the amino acid. These monodispersed water soluble AuNPs synthesized using non-toxic, naturally occurring α-amino acids as reducing and capping/stabilizing agents serve as a remarkable example of green chemistry.

  14. Novel and efficient one-pot five- and six-component reactions for the stereoselective synthesis of highly functionalized enaminones and dithiocarbamates.

    PubMed

    Bararjanian, Morteza; Balalaie, Saeed; Rominger, Frank; Movassagh, Barahman; Bijanzadeh, Hamid Reza

    2011-05-01

    Efficient methods for stereoselective synthesis of polyfunctional (E)-enaminones and (Z)-dithiocarbamates via one-pot five- and six-component sequential Ugi/Nucleophilic addition reactions are described. High yields and high bond forming efficiency, and simple operations are the advantages of this method. PMID:21072590

  15. Gold Nanoparticles Supported on a Layered Double Hydroxide as Efficient Catalysts for the One-Pot Synthesis of Flavones.

    PubMed

    Yatabe, Takafumi; Jin, Xiongjie; Yamaguchi, Kazuya; Mizuno, Noritaka

    2015-11-01

    Flavones are a class of natural products with diverse biological activities and have frequently been synthesized by step-by-step procedures using stoichiometric amounts of reagents. Herein, a catalytic one-pot procedure for the synthesis of flavone and its derivatives is developed. In the presence of gold nanoparticles supported on a Mg-Al layered double hydroxide (Au/LDH), various kinds of flavones can be synthesized starting from 2'-hydroxyacetophenones and benzaldehydes (or benzyl alcohols). The present one-pot procedure consists of a sequence of several reactions, and Au/LDH can catalyze all these different types of reactions. The catalysis is shown to be truly heterogeneous, and Au/LDH can be readily recovered and reused.

  16. One-pot synthesis of (-)-Ambrox.

    PubMed

    Yang, Shaoxiang; Tian, Hongyu; Sun, Baoguo; Liu, Yongguo; Hao, Yanfeng; Lv, Yanyu

    2016-01-01

    (-)-Ambrox is recognised as the prototype of all ambergris odorants. Widely used in perfumery, (-)-Ambrox is an important ingredient due to its unique scent and excellent fixative function. An environmentally friendly and practical preparation of (-)-Ambrox is still unavailable at present although a lot of attention has been paid to this hot research topic for many years. A one-pot synthesis of (-)-Ambrox was studied starting from (-)-sclareol through oxidation with hydrogen peroxide in the presence of a quaternary ammonium phosphomolybdate catalyst {[C5H5NC16H33] [H2PMo12O40]}, which gave the product a 20% overall yield. PMID:27581945

  17. Efficient Palladium-Assisted One-Pot Deprotection of (Acetamidomethyl)Cysteine Following Native Chemical Ligation and/or Desulfurization To Expedite Chemical Protein Synthesis.

    PubMed

    Maity, Suman Kumar; Jbara, Muhammad; Laps, Shay; Brik, Ashraf

    2016-07-01

    The acetamidomethyl (Acm) moiety is a widely used cysteine protecting group for the chemical synthesis and semisynthesis of peptide and proteins. However, its removal is not straightforward and requires harsh reaction conditions and additional purification steps before and after the removal step, which extends the synthetic process and reduces the overall yield. To overcome these shortcomings, a method for rapid and efficient Acm removal using Pd(II) complexes in aqueous medium is reported. We show, for the first time, the assembly of three peptide fragments in a one-pot fashion by native chemical ligation where the Acm moiety was used to protect the N-terminal Cys of the middle fragment. Importantly, an efficient synthesis of the ubiquitin-like protein UBL-5, which contains two native Cys residues, was accomplished through the one-pot operation of three key steps, namely ligation, desulfurization, and Acm deprotection, highlighting the great utility of the new approach in protein synthesis.

  18. An efficient and scalable one-pot double Michael addition-Dieckmann condensation for the synthesis of 4,4-disubstituted cyclohexane beta-keto esters.

    PubMed

    DeGraffenreid, Michael R; Bennett, Sarah; Caille, Sebastien; Gonzalez-Lopez de Turiso, Felix; Hungate, Randall W; Julian, Lisa D; Kaizerman, Jacob A; McMinn, Dustin L; Rew, Yosup; Sun, Daqing; Yan, Xuelei; Powers, Jay P

    2007-09-14

    A simple, scalable, and efficient one-pot methodology for the synthesis of 4,4-disubstituted cyclohexane beta-keto esters from benzylic nitriles or esters and methyl acrylate promoted by potassium tert-butoxide is described. The process relies on a tandem double Michael addition-Dieckmann condensation reaction, which results in the formation of three discrete carbon-carbon bonds in a single pot, including a quaternary center. The method allows for the convenient and rapid synthesis of a variety of 4-aryl-4-cyano-2-carbomethoxycyclohexanone and 4-aryl-2,4-biscarbomethoxycyclohexanone building blocks for use in natural products synthesis and medicinal chemistry. PMID:17696402

  19. One-pot facile synthesis of branched Ag-ZnO heterojunction nanostructure as highly efficient photocatalytic catalyst

    NASA Astrophysics Data System (ADS)

    Huang, Qingli; Zhang, Qitao; Yuan, Saisai; Zhang, Yongcai; Zhang, Ming

    2015-10-01

    In this paper, the branched Ag-ZnO heterojunction nanostructure and the branched ZnO were synthesized successfully by a facile, green and one-pot hydrothermal method. Such branched heterojunction and the comparing branched pure ZnO were characterized by X-ray diffraction, field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), energy-dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), photoluminescence spectroscopy (PL) and UV-vis diffuse reflectance spectra (DRS). The photocatalytic degradation of RhB aqueous solution and acetaldehyde (CH3CHO) gas results both showed that the branched Ag-ZnO heterojunction possessed the enhanced photocatalytic properties in comparison to the branched ZnO and Ag-ZnO counterparts due to its special interface structures and fast separation of its photogenerated charge carriers. This method is simple, feasible and can provide an important clue for synthesis and application of other branched metal/semiconductor heterojunction nanostructures.

  20. Transition metal-free one-pot synthesis of nitrogen-containing heterocycles.

    PubMed

    Kumari, Simpal; Kishore, Dharma; Paliwal, Sarvesh; Chauhan, Rajani; Dwivedi, Jaya; Mishra, Aakanksha

    2016-02-01

    One-pot heterocyclic synthesis is an exciting research area as it can open routes for the development of otherwise complex transformations in organic synthesis. Heterocyclic compounds show wide spectrum of applications in medicinal chemistry, chemical biology, and materials science. These heterocycles can be generated very efficiently through highly economical and viable routes using one-pot synthesis. In particular, the metal-free one-pot synthetic protocols are highly fascinating due to several advantages for the industrial production of heterocyclic frameworks. This comprehensive review is devoted to the transition metal-free one-pot synthesis of nitrogen-containing heterocycles from the period 2010-2013.

  1. p-Sulfonic Acid Calix[4]arene as an Efficient Catalyst for One-Pot Synthesis of Pharmaceutically Significant Coumarin Derivatives under Solvent-Free Condition

    PubMed Central

    Tashakkorian, Hamed; Lakouraj, Moslem Mansour; Rouhi, Mona

    2015-01-01

    One-pot and efficient protocol for preparation of some potent pharmaceutically valuable coumarin derivatives under solvent-free condition via direct coupling using biologically nontoxic organocatalyst, calix[4]arene tetrasulfonic acid (CSA), was introduced. Calix[4]arene sulfonic acid has been incorporated lately as a magnificent and recyclable organocatalyst for the synthesis of some organic compounds. Nontoxicity, solvent-free conditions, good-to-excellent yields for pharmaceutically significant structures, and especially ease of catalyst recovery make this procedure valuable and environmentally benign. PMID:26798517

  2. Copper ferrite nanoparticles: an efficient and reusable nanocatalyst for a green one-pot, three-component synthesis of spirooxindoles in water.

    PubMed

    Bazgir, Ayoob; Hosseini, Ghaffar; Ghahremanzadeh, Ramin

    2013-10-14

    A green reaction of isatins, active cyanomethanes, and cyclic 1,3-dicarbonyl derivatives for the efficient and simple one-pot three-component synthesis of spirooxindole fused heterocycles in refluxing water by use of magnetically recoverable and reusable catalyst is reported. The features of this procedure are, the use of magnetically recoverable and reusable catalyst, mild reaction conditions, high to excellent product yields, operational simplicity, and easy workup procedures. Most importantly of all, easy magnetic separation of the catalyst eliminates the requirement of catalyst filtration after completion of the reaction. Furthermore, the catalyst remained highly active even after 5 repeated uses. PMID:24050156

  3. ZnO Nanoparticles as an Efficient, Heterogeneous, Reusable, and Ecofriendly Catalyst for Four-Component One-Pot Green Synthesis of Pyranopyrazole Derivatives in Water

    PubMed Central

    Sachdeva, Harshita; Saroj, Rekha

    2013-01-01

    An extremely efficient catalytic protocol for the synthesis of a series of pyranopyrazole derivatives developed in a one-pot four-component approach in the presence of ZnO nanoparticles as heterogeneous catalyst using water as a green solvent is reported. Greenness of the process is well instituted as water is exploited both as reaction media and medium for synthesis of catalyst. The ZnO nanoparticles exhibited excellent catalytic activity, and the proposed methodology is capable of providing the desired products in good yield (85–90%) and short reaction time. After reaction course, ZnO nanoparticles can be recycled and reused without any apparent loss of activity which makes this process cost effective and hence ecofriendly. All the synthesized compounds have been characterized on the basis of elemental analysis, IR, 1H NMR, and 13C NMR spectral studies. PMID:24282386

  4. One pot synthesis of new hybrid versatile nanocarrier exhibiting efficient stability in biological environment for use in photodynamic therapy.

    PubMed

    Thienot, Edouard; Germain, Matthieu; Piejos, Kelthoum; Simon, Virginie; Darmon, Audrey; Marill, Julie; Borghi, Elsa; Levy, Laurent; Hochepied, Jean-François; Pottier, Agnès

    2010-07-01

    A new versatile hybrid nanocarrier has been designed using a "soft chemistry" synthesis, to efficiently encapsulate a photosensitizer - the protoporphyrin IX (Pp IX) - while preserving its activity intact in biological environment for advantageous use in photodynamic therapy (PDT). The synthesized Pp IX silica-based nanocarriers show to be spherical in shape and highly monodisperse with size extending from 10 nm up to 200 nm according to the synthesis procedure. Upon laser irradiation, the entrapped Pp IX shows to efficiently deliver reactive oxygen species (ROS) which are responsible for damaging tumor tissues. The ability of Pp IX silica-based nanocarriers to induce tumor cell death has been tested successfully in vitro. The stability of the Pp IX silica-based nanocarriers has been followed by UV-vis absorption and fluorescence emission in aqueous media and in 100% mouse serum media. The flexibility of the nanocarrier silica core has been examined as the key parameter to tune the Pp IX stability in biological environment. Indeed, an additional biocompatible inorganic surface coating performed on the Pp IX silica-based nanocarriers to produce an optimized bilayer coating demonstrates to significantly enhance the Pp IX stabilization in biological environments. Such versatile hybrid nanocarriers open new perspectives for PDT. PMID:20456971

  5. One-Pot Synthesis of Hydrophobically Modified Iminosugar C-Alkynylglycosides: Facile Synthesis of Polyhydroxy Tetrahydroindolizines.

    PubMed

    Senthilkumar, Soundararasu; Prasad, Sure Siva; Das, Amrita; Baskaran, Sundarababu

    2015-11-01

    A mild and efficient one-pot method has been developed for the stereoselective synthesis of structurally diverse novel iminosugar C-alkynylglycosides. The generality of this methodology has been demonstrated with a wide variety of amines and copper acetylides. This one-pot method has been exploited in the synthesis of new class of DNA cross-linking agents, polyhydroxy 1-vinyl-tetrahydroindolizine derivatives.

  6. An efficient one-pot synthesis of thiochromeno[3,4-d]pyrimidines derivatives: Inducing ROS dependent antibacterial and anti-biofilm activities.

    PubMed

    Suresh, Lingala; Sagar Vijay Kumar, P; Poornachandra, Y; Ganesh Kumar, C; Chandramouli, G V P

    2016-10-01

    An efficient synthesis of thiochromeno[3,4-d]pyrimidine derivatives has been achieved successfully via a one-pot three-component reaction of thiochrome-4-one, aromatic aldehyde and thiourea in the presence of 1-butyl-3-methyl imidazolium hydrogen sulphate [Bmim]HSO4. This new protocol has the advantages of environmental friendliness, high yields, short reaction times, and convenient operation. Furthermore, among all the tested derivatives, compounds 4b and 4c exhibited promising antibacterial, minimum bactericidal concentration and anti-biofilm activities against Staphylococcus aureus MTCC 96, Staphylococcus aureus MLS16 MTCC 2940 and Bacillus subtilis MTCC 121. The compound 4c also showed promising intracellular ROS accumulation in Staphylococcus aureus MLS16 MTCC 2940 comparable to that of ciprofloxacin resulting in apoptotic cell death of the bacterium. PMID:27522461

  7. One-pot synthesis of gold-palladium@palladium core-shell nanoflowers as efficient electrocatalyst for ethanol electrooxidation

    NASA Astrophysics Data System (ADS)

    Qiu, Xiaoyu; Dai, Yuxuan; Tang, Yawen; Lu, Tianhong; Wei, Shaohua; Chen, Yu

    2015-03-01

    In this work, a simple polyallylamine-assisted water-based synthesis is successfully used to synthesize high-quality gold-palladium@palladium (Au-Pd@Pd) core-shell nanoflowers. Transmission electron microscopy, X-ray powder diffraction, element mapping, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy techniques are used to characterize the morphology, structure and composition of Au-Pd@Pd core-shell nanoflowers. The as-prepared Au-Pd@Pd core-shell nanoflowers exhibit significantly enhanced electrocatalytic activity for the ethanol oxidation reaction (EOR) in basic medium compared with commercial Pd black. In addition, Au-Pd@Pd core-shell nanoflowers also show higher durability for the EOR than commercial Pd black.

  8. Graphite-supported perchloric acid (HClO4-C): an efficient and recyclable heterogeneous catalyst for the one-pot synthesis of amidoalkyl naphthols.

    PubMed

    Lei, Zhen-Kai; Xiao, Li; Lu, Xiao-Quan; Huang, He; Liu, Chen-Jiang

    2013-01-01

    An efficient and direct protocol for the preparation of amidoalkylnaphthols employing a multi-component, one-pot condensation reaction of 2-naphthol, aromatic aldehydes and acetamide or benzamide in the presence of graphite supported perchloric acid under solvent-free conditions is described. The thermal solvent-free procedure offers advantages such as simple work-up, shorter reaction times and higher product yields, and the catalyst exhibited remarkable reactivity and can be recycled.

  9. Graphite-supported perchloric acid (HClO4-C): an efficient and recyclable heterogeneous catalyst for the one-pot synthesis of amidoalkyl naphthols.

    PubMed

    Lei, Zhen-Kai; Xiao, Li; Lu, Xiao-Quan; Huang, He; Liu, Chen-Jiang

    2013-01-01

    An efficient and direct protocol for the preparation of amidoalkylnaphthols employing a multi-component, one-pot condensation reaction of 2-naphthol, aromatic aldehydes and acetamide or benzamide in the presence of graphite supported perchloric acid under solvent-free conditions is described. The thermal solvent-free procedure offers advantages such as simple work-up, shorter reaction times and higher product yields, and the catalyst exhibited remarkable reactivity and can be recycled. PMID:23358323

  10. Designed copper-amine complex as an efficient template for one-pot synthesis of Cu-SSZ-13 zeolite with excellent activity for selective catalytic reduction of NOx by NH3.

    PubMed

    Ren, Limin; Zhu, Longfeng; Yang, Chengguang; Chen, Yanmei; Sun, Qi; Zhang, Haiyan; Li, Caijin; Nawaz, Faisal; Meng, Xiangju; Xiao, Feng-Shou

    2011-09-21

    Low-cost copper-amine complex was rationally designed to be a novel template for one-pot synthesis of Cu-SSZ-13 zeolites. Proper confirmation and appropriate size make this complex fit well with CHA cages as an efficient template. The products exhibit superior catalytic performance on NH(3)-SCR reaction. PMID:21625721

  11. Efficient Catalyst One-Pot Synthesis of 7-(Aryl)-10,10-dimethyl-10,11-dihydrochromeno[4,3-b]chromene-6,8(7H,9H)-dione Derivatives Complemented by Antibacterial Activity

    PubMed Central

    Al-Majedy, Yasameen K.; Kadhum, Abdul Amir H.; Mohamad, Abu Bakar

    2016-01-01

    The problem of bacteria resistance to many known agents has inspired scientists and researchers to discover novel efficient antibacterial drugs. Three rapid, clean, and highly efficient methods were developed for one-pot synthesis of 7-(aryl)-10,10-dimethyl-10,11-dihydrochromeno[4,3-b]chromene-6,8(7H,9H)-dione derivatives. Three components are condensed in the synthesis, 4-hydroxycoumarin, 5,5-dimethyl-1,3-cyclohexanedione, and aromatic aldehydes, using tetrabutylammonium bromide (TBAB), diammonium hydrogen phosphate (DAHP), or ferric chloride (FeCl3), respectively. Each method has different reaction mechanisms according to the catalyst. The present methods have advantages, including one-pot synthesis, excellent yields, short reaction times, and easy isolation of product. All catalysts utilized in our study could be reused several times without losing their catalytic efficiency. All synthesized compounds were fully characterized and evaluated for their antibacterial activity. PMID:27563671

  12. Efficient Catalyst One-Pot Synthesis of 7-(Aryl)-10,10-dimethyl-10,11-dihydrochromeno[4,3-b]chromene-6,8(7H,9H)-dione Derivatives Complemented by Antibacterial Activity.

    PubMed

    Al-Majedy, Yasameen K; Al-Amiery, Ahmed A; Kadhum, Abdul Amir H; Mohamad, Abu Bakar

    2016-01-01

    The problem of bacteria resistance to many known agents has inspired scientists and researchers to discover novel efficient antibacterial drugs. Three rapid, clean, and highly efficient methods were developed for one-pot synthesis of 7-(aryl)-10,10-dimethyl-10,11-dihydrochromeno[4,3-b]chromene-6,8(7H,9H)-dione derivatives. Three components are condensed in the synthesis, 4-hydroxycoumarin, 5,5-dimethyl-1,3-cyclohexanedione, and aromatic aldehydes, using tetrabutylammonium bromide (TBAB), diammonium hydrogen phosphate (DAHP), or ferric chloride (FeCl3), respectively. Each method has different reaction mechanisms according to the catalyst. The present methods have advantages, including one-pot synthesis, excellent yields, short reaction times, and easy isolation of product. All catalysts utilized in our study could be reused several times without losing their catalytic efficiency. All synthesized compounds were fully characterized and evaluated for their antibacterial activity. PMID:27563671

  13. An efficient one-pot two catalyst system in the construction of 2-substituted benzimidazoles: synthesis of benzimidazo[1,2-c]quinazolines.

    PubMed

    Cimarelli, Cristina; Di Nicola, Matteo; Diomedi, Simone; Giovannini, Riccardo; Hamprecht, Dieter; Properzi, Roberta; Sorana, Federico; Marcantoni, Enrico

    2015-12-28

    The benzimidazole core is a common moiety in a large number of natural products and pharmacologically active small molecules. The synthesis of novel benzimidazole derivatives remains a main focus in medicinal research. In continuation of the efforts towards Ce(III) catalysts for organic transformations, we observed for the first time the activity of the iodide ion and copper cation in activating CeCl3·7H2O in the selective formation of prototypical 2-substituted benzimidazoles. The one-pot CeCl3·7H2O-CuI catalytic system procedure includes the cyclo-dehydrogenation of aniline Schiff's bases, generated in situ from the condensation of 1,2-phenylenediamine and aldehydes, followed by the oxidation with iodine, which works as a hydrogen sponge. Mild reaction conditions, good to excellent yields, and clean reactions make the procedure a useful contribution to the synthesis of biologically active fused heterocycles containing benzimidazoquinazolines. PMID:26477673

  14. Combinatorial one-pot chemoenzymatic synthesis of heparin.

    PubMed

    Bhaskar, Ujjwal; Li, Guoyun; Fu, Li; Onishi, Akihiro; Suflita, Mathew; Dordick, Jonathan S; Linhardt, Robert J

    2015-05-20

    Contamination in heparin batches during early 2008 has resulted in a significant effort to develop a safer bioengineered heparin using bacterial capsular polysaccharide heparosan and recombinant enzymes derived from the heparin/heparan sulfate biosynthetic pathway. This requires controlled chemical N-deacetylation/N-sulfonation of heparosan followed by epimerization of most of its glucuronic acid residues to iduronic acid and O-sulfation of the C2 position of iduronic acid and the C3 and C6 positions of the glucosamine residues. A combinatorial study of multi-enzyme, one-pot, in vitro biocatalytic synthesis, carried out in tandem with sensitive analytical techniques, reveals controlled structural changes leading to heparin products similar to animal-derived heparin active pharmaceutical ingredients. Liquid chromatography-mass spectrometry and nuclear magnetic resonance spectroscopy analysis confirms an abundance of heparin's characteristic trisulfated disaccharide, as well as 3-O-sulfo containing residues critical for heparin binding to antithrombin III and its anticoagulant activity. The bioengineered heparins prepared using this simplified one-pot chemoenzymatic synthesis also show in vitro anticoagulant activity.

  15. One-pot green synthesis of Prussian blue nanocubes decorated reduced graphene oxide using mushroom extract for efficient 4-nitrophenol reduction.

    PubMed

    Chen, Ruixue; Zhang, Qiuping; Gu, Yue; Tang, Liu; Li, Cong; Zhang, Zhiquan

    2015-01-01

    One-pot green approach to the synthesis of Prussian blue nanocubes/reduced graphene oxide (PBNCs/RGO) nanocomposite had been attempted. It was based on the extract of mushroom with K3[Fe(CN)6] and graphene oxide (GO) as precursors, where the reduction of GO and the deposition of PBNCs occurred simultaneously. The obtained nanocomposite was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy and electrochemical techniques. With the introduction of β-cyclodextrin (β-CD), the β-CD/PBNCs/RGO system showed linear behavior in the range from 0.01 to 700 μM for 4-nitrophenol with a low detection limit of 2.34 nM (S/N=3).

  16. One-Pot Template-Free Synthesis of Cu-MOR Zeolite toward Efficient Catalyst Support for Aerobic Oxidation of 5-Hydroxymethylfurfural under Ambient Pressure.

    PubMed

    Zhang, Wei; Xie, Jingyan; Hou, Wei; Liu, Yangqing; Zhou, Yu; Wang, Jun

    2016-09-01

    Supported catalysts are widely studied, and exploring new promising supports is significant to access more applications. In this work, novel copper-containing MOR-type zeolites Cu-MOR were synthesized in a one-pot template-free route and served as efficient supports for vanadium oxide. In the heterogeneous oxidation of 5-hydroxymethylfurfural (HMF) to 2,5-diformylfuran (DFF) with molecular oxygen (O2) under ambient pressure, the obtained catalyst demonstrated high yield (91.5%) and good reusability. Even under the ambient air pressure, it gave a DFF yield of 72.1%. Structure-activity relationship analysis indicated that the strong interaction between the framework Cu species and the guest V sites accounted for the remarkable performance. This work reveals that the Cu-MOR zeolite uniquely acts as the robust support toward well-performed non-noble metal heterogeneous catalyst for biomass conversion. PMID:27523255

  17. One-pot synthesis of NiFe layered double hydroxide/reduced graphene oxide composite as an efficient electrocatalyst for electrochemical and photoelectrochemical water oxidation

    NASA Astrophysics Data System (ADS)

    Youn, Duck Hyun; Park, Yoon Bin; Kim, Jae Young; Magesh, Ganesan; Jang, Youn Jeong; Lee, Jae Sung

    2015-10-01

    As an efficient non-precious metal catalyst for oxygen evolution reaction (OER) in electrochemical and photoelectrochemical water splitting, NiFe layered double hydroxide (LDH)/reduced graphene oxide (NiFe/RGO) composite is synthesized by a simple solvothermal method in one-pot. NiFe LDHs are uniformly deposited on RGO layers of high electrical conductivity and large surface area. In electrochemical water splitting, NiFe/RGO shows superior OER performance compared to bare NiFe and reference IrO2 with a lower benchmark η10 value (required overpotential to drive 10 mA cm-2) of 0.245 V. Furthermore, NiFe/RGO substantially increases the performance of a hematite photoanode in photoelectrochemical water oxidation, demonstrating its potential as an OER co-catalyst for photoelectrodes.

  18. One-pot synthesis of (−)-Ambrox

    PubMed Central

    Yang, Shaoxiang; Tian, Hongyu; Sun, Baoguo; Liu, Yongguo; Hao, Yanfeng; Lv, Yanyu

    2016-01-01

    (−)-Ambrox is recognised as the prototype of all ambergris odorants. Widely used in perfumery, (−)-Ambrox is an important ingredient due to its unique scent and excellent fixative function. An environmentally friendly and practical preparation of (−)-Ambrox is still unavailable at present although a lot of attention has been paid to this hot research topic for many years. A one-pot synthesis of (−)-Ambrox was studied starting from (−)-sclareol through oxidation with hydrogen peroxide in the presence of a quaternary ammonium phosphomolybdate catalyst {[C5H5NC16H33] [H2PMo12O40]}, which gave the product a 20% overall yield. PMID:27581945

  19. One-pot solvothermal synthesis of ordered intermetallic Pt2In3 as stable and efficient electrocatalyst towards direct alcohol fuel cell application

    NASA Astrophysics Data System (ADS)

    Jana, Rajkumar; Peter, Sebastian C.

    2016-10-01

    Ordered intermetallic Pt2In3 nanoparticles have been synthesized by superhydride reduction of K2PtCl4 and InCl3.xH2O precursors using facile, one-pot solvothermal method. We report surfactant free solvothermal synthesis of a novel ordered Pt2In3 intermetallic nanoparticles for the first time. The structure and morphology of the catalyst has been confirmed by powder X-ray diffraction, transmission electron microscopy, field emission scanning electron microscopy, energy-dispersive spectrometry and X-ray photoelectron spectroscopy. The electrocatalytic properties of the catalysts have been investigated by cyclic voltammetry and chronoamperometry. The as prepared Pt2In3 catalyst exhibit far superior electrocatalytic activity and stability towards alcohol oxidation over commercial Pt/C. The specific activity of as synthesized catalyst was found to be ~3.2 and ~2.3 times higher than commercial Pt/C for methanol and ethanol oxidation, respectively. This improved activity and durability of the Pt2In3 nanoparticles can make the catalyst an ideal catalyst candidate for direct alcohol fuel cell.

  20. General and efficient one-pot synthesis of novel sugar/heterocyclic(aryl) 1,2-diketones from sugar terminal alkynes by Sonogashira/tetra-n- butylammonium permanganate oxidation.

    PubMed

    Zhang, Fuyi; Wu, Xiaopei; Wang, Liming; Liu, Hong; Zhao, Yufen

    2015-11-19

    A new approach for one-pot synthesis of novel sugar/heterocyclic(aryl) 1,2-diketones has been achieved by the reaction of various sugar terminal alkynes with heterocyclic(aryl) iodides at room temperature. This one-pot protocol includes Sonogashira coupling and mild n-Bu4NMnO4 oxidation reaction. This method is mild, general and efficient. Fifty-six examples have been given and the sugar/heterocyclic(aryl) 1,2-diketones were obtained in 71-94% yields. The sugar terminal alkynes include 9 structurally different sugars in pyranose, furanose, and acyclic form which have various protecting groups, sensitive groups, and sterically bulky substituents. The heterocyclic(aryl) iodides include sterically bulky heterocyclic compounds and iodobenzenes with electron-donating, electron-neutral, and electron-withdrawing substituents.

  1. One-pot synthesis of CdS nanocrystals hybridized with single-layer transition-metal dichalcogenide nanosheets for efficient photocatalytic hydrogen evolution.

    PubMed

    Chen, Junze; Wu, Xue-Jun; Yin, Lisha; Li, Bing; Hong, Xun; Fan, Zhanxi; Chen, Bo; Xue, Can; Zhang, Hua

    2015-01-19

    Exploration of low-cost and earth-abundant photocatalysts for highly efficient solar photocatalytic water splitting is of great importance. Although transition-metal dichalcogenides (TMDs) showed outstanding performance as co-catalysts for the hydrogen evolution reaction (HER), designing TMD-hybridized photocatalysts with abundant active sites for the HER still remains challenge. Here, a facile one-pot wet-chemical method is developed to prepare MS2-CdS (M=W or Mo) nanohybrids. Surprisedly, in the obtained nanohybrids, single-layer MS2 nanosheets with lateral size of 4-10 nm selectively grow on the Cd-rich (0001) surface of wurtzite CdS nanocrystals. These MS2-CdS nanohybrids possess a large number of edge sites in the MS2 layers, which are active sites for the HER. The photocatalytic performances of WS2-CdS and MoS2-CdS nanohybrids towards the HER under visible light irradiation (>420 nm) are about 16 and 12 times that of pure CdS, respectively. Importantly, the MS2-CdS nanohybrids showed enhanced stability after a long-time test (16 h), and 70% of catalytic activity still remained.

  2. One-pot synthesis of C₁₈-functionalized core-shell magnetic mesoporous silica composite as efficient sorbent for organic dye.

    PubMed

    Zhang, Xiaole; Zeng, Tao; Wang, Saihua; Niu, Hongyun; Wang, Xiaoke; Cai, Yaqi

    2015-06-15

    In this work, a facile one-pot strategy was proposed for the synthesis of C18-functionalized core-shell magnetic mesoporous silica composite (Fe3O4/mSiO2-C18). The Fe3O4/mSiO2-C18 composite, with an average size of 80 nm and a functionalized mesoporous silica shell of about 30 nm in thickness, has excellent adsorption ability toward methylene blue dye (MB) due to the large surface area (303 m(2) g(-1)) and the abundant hydrophobic C18 groups. The adsorption equilibrium was achieved within 20 min and the adsorption behavior of MB on Fe3O4/mSiO2-C18 composite fitted the pseudo-second-order kinetic model well (k2=1.29×10(-2) g mg(-1) min(-1), q(e)=144.72 mg g(-1), h(o)=270.27 mg g(-1) min(-1) under 25 °C and an initial MB concentration of 10 mg L(-1)). Langmuir and Freundlich isothermal adsorption models can both be used to describe the adsorption process and the maximum Langmuir adsorption capacity of MB on Fe3O4/mSiO2-C18 at 25 °C and pH 7.5 is 363.64 mg g(-1). Thermodynamic parameters show that the adsorption reaction is exothermic and spontaneous (ΔH(0)=-63.49 kJ mol(-1), ΔG(0)=-7.80 kJ mol(-1)). Ionic strength and pH affected the adsorption slightly. In addition, the MB adsorbed sorbent can be readily separated from water solution by an external magnet because of the high magnetic saturation value (22.62 emu g(-1)). After being regenerated by treatment with acidic methanol, the sorbent could be reused for at least 5 cycles with a little decrease in adsorption capacity.

  3. One-Pot Regiospecific Synthesis of Quinoxalines via a CH2-Extrusion Reaction.

    PubMed

    Shen, Jinhai; Wang, Xiangdong; Lin, Xing; Yang, Zhenhui; Cheng, Guolin; Cui, Xiuling

    2016-03-18

    A convenient "one-pot" regiospecific synthesis of substituted quinoxalines from o-phenylenediamines and ynones under metal-free conditions has been developed. An intermolecular Michael addition reaction, a dehydration condensation, and a base-promoted C-α-CH2-extrusion were involved in this procedure, which features high regioselectivity, efficiency, and environmental friendliness. Various quinoxalines were provided in up to 95% yield for 33 examples. PMID:26925522

  4. A green and efficient protocol for the synthesis of dihydropyrano[2,3-c]pyrazole derivatives via a one-pot, four component reaction by grinding method

    PubMed Central

    Ambethkar, Sethurajan; Padmini, Vediappen; Bhuvanesh, Nattamai

    2014-01-01

    An efficient grinding protocol for the synthesis of dihydropyrano[2,3-c]pyrazole derivatives from acetylene ester, hydrazine hydrate, aryl aldehydes and malononitrile under solvent free conditions has been achieved with excellent yields. The structures of the synthesized compounds were deduced by spectroscopic techniques and the compounds were further evaluated for their in vitro antioxidant and antimicrobial activities. PMID:26644936

  5. One-pot, green, rapid synthesis of flowerlike gold nanoparticles/reduced graphene oxide composite with regenerated silk fibroin as efficient oxygen reduction electrocatalysts.

    PubMed

    Xu, Shengjie; Yong, Liu; Wu, Peiyi

    2013-02-01

    Flowerlike gold nanoparticles (Au NPs)/reduced graphene oxide (RGO) composites were fabricated by a facile, one-pot, environmentally friendly method in the presence of regenerated silk fibroin (RSF). The influences of reaction time, temperature, and HAuCl(4): RGO ratio on the morphology of Au NPs loaded on RGO sheets were discussed and a tentative mechanism for the formation of flowerlike Au NPs/RGO composite was proposed. In addition, the flowerlike Au NPs/RGO composite showed superior catalytic performance for oxygen reduction reaction (ORR) to Au/RGO composites with other morphologies. Our work provides an alternative facile and green approach to synthesize functional metal/RGO composites.

  6. Efficient one-pot cyclization/folding of Rhesus θ-defensin-1 (RTD-1)

    PubMed Central

    Aboye, Teshome L.; Li, Yilong; Majumder, Subhabrata; Hao, Jinfeng; Shekhtman, Alexander; Camarero, Julio A.

    2012-01-01

    We report an efficient approach for the chemical synthesis of Rhesus θ-defensin-1 (RTD-1) using Fmoc-based solid-phase peptide synthesis in combination with an intramolecular version of native chemical ligation. The corresponding linear thioester precursor was cyclized and folded in a one-pot reaction using reduced glutathione. The reaction was extremely efficiently yielding natively folded RTD-1 with minimal or no purification at all. This approach is fully compatible with the high throughput production of chemical libraries using this peptide scaffold. PMID:22425570

  7. Palladium-catalyzed one-pot three- or four-component coupling of aryl iodides, alkynes, and amines through C-N bond cleavage: efficient synthesis of indole derivatives.

    PubMed

    Hao, Wei; Geng, Weizhi; Zhang, Wen-Xiong; Xi, Zhenfeng

    2014-02-24

    An efficient synthesis of N-substituted indole derivatives was realized by combining the Pd-catalyzed one-pot multicomponent coupling approach with cleavage of the C(sp(3))-N bonds. Three or four components of aryl iodides, alkynes, and amines were involved in this coupling process. The cyclopentadiene-phosphine ligand showed high efficiency. A variety of aryl iodides, including cyclic and acyclic tertiary amino aryl iodides, and substituted 1-bromo-2-iodobenzene derivatives could be used. Both symmetric and unsymmetric alkynes substituted with alkyl, aryl, or trimethylsilyl groups could be applied. Cyclic secondary amines such as piperidine, morpholine, 4-methylpiperidine, 1-methylpiperazine, 2-methylpiperidine, and acyclic amines including secondary and primary amines all showed good reactivity. Further application of the resulting indole derivatives was demonstrated by the synthesis of benzosilolo[2,3-b]indole.

  8. Ag(I)-triggered one-pot synthesis of Ag nanoparticles onto natural nanorods as a multifunctional nanocomposite for efficient catalysis and adsorption.

    PubMed

    Tian, Guangyan; Wang, Wenbo; Mu, Bin; Kang, Yuru; Wang, Aiqin

    2016-07-01

    A multifunctional palygorskite/polyaniline/Ag nanoparticles (PAL/PANI/AgNPs) nanocomposite was prepared at room temperature using a simple one-pot in-situ polymerization reaction of aniline monomers triggered by Ag(I) on the surface of natural PAL nanorods. Ag(I) served as both the oxidant and the precursor of the AgNPs, which initiated the polymerization of aniline monomers on PAL nanorods while simultaneously being reduced to form Ag(0) nanoparticles (AgNPs). The in-situ formed AgNPs were evenly distributed on the surface of the PAL nanorods because the interfacial effect of PAL prevents their aggregation. The density and size of the AgNPs and the catalytic activity of the nanocomposites could be controlled by altering the molar ratio of aniline to Ag(I). The performance evaluation revealed that the nanocomposites could be used as highly active catalysts, which rapidly catalyzed the reduction of 4-nitrophenol (4-NP) within 2min and Congo red (CR) within 10min. The nanocomposites are also an effective adsorbent for H2PO4(-) able to remove 99.40% of H2PO4(-) (only 61.77% for raw PAL) from a solution with an initial concentration of 50mg/L. This multifunctional nanocomposite synthesized by a simple one-pot approach is a promising material for environmental applications.

  9. An efficient Bi(NO3)3 x 5H2O catalyzed multi component one-pot synthesis of novel naphthyridines.

    PubMed

    Ravikumar Naik, Tangali R; Bhojya Naik, Halehatty S

    2008-05-01

    An efficient and environmentally friendly multicomponent synthesis of substituted 1,8-naphthyridines catalyzed by bismuth(III) nitrate pentahydrate [Bi(NO3)3 x 5H2O] under solvent-free microwave irradiation is described. This procedure has such advantages as short reaction time, high yields, and simple workup. The catalyst could be reused several times, keeping its initial activity recycled reactions. PMID:18587659

  10. Efficient one-pot synthesis of trans-Pt(II)(salicylaldimine)(4-picoline)Cl complexes: effective agents for enhanced expression of p53 tumor suppressor genes.

    PubMed

    Rahman, Faiz-Ur; Ali, Amjad; Guo, Rong; Wang, Wei-Kun; Wang, Hui; Li, Zhan-Ting; Lin, Yuejian; Zhang, Dan-Wei

    2015-06-01

    A series of trans-Pt(II)(salicylaldimine)(4-picoline)Cl complexes were synthesized in 78-87% yield using a one-pot procedure from commercially available precursors. The structures of these complexes were characterized by (1)H, (19)F and (13)C NMR spectroscopy, HRMS (ESI) as well as single crystal X-ray analysis. Bioactivity investigations including bio-assay, time- and dose-dependent, cell cycle progression study, caspase 3 and 9 apoptosis marker assay and DNA interaction using pBR322 plasmid DNA by gel electrophoresis were performed. The results indicated that the complexes showed promising in vitro cytotoxicity in MCF-7 and A549 cancer cell lines. Moreover these complexes enhanced the expression of p53 tumor suppressor gene family members such as p63 and p73.

  11. Efficient one-pot synthesis of pyrido[2,3-d]pyrimidines catalyzed by nanocrystalline MgO in water

    NASA Astrophysics Data System (ADS)

    Rad, Amaneh Mossafaii; Mokhtary, Masoud

    2015-04-01

    The direct three-component condensation of 6-aminouracil, 6-amino-2-thiouracil or 6-amino-1,3-dimethyluracil, with arylaldehydes and malononitrile to generate a series of pyrido[2,3-d]pyrimidine derivatives has been carried out over nanocrystalline MgO with high efficiency in water as a green solvent at 80 °C. The morphology and structure of the nanocrystalline MgO were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The results confirmed the nanocrystalline MgO particle size is approximately 50 nm. This methodology offers significant improvements for the synthesis of pyrido[2,3-d]pyrimidine derivatives with regard to the yield of products, simplicity in operation, and green aspects by avoiding toxic catalysts and solvents.

  12. One-pot synthesis of metal-carbon nanotubes network hybrids as highly efficient catalysts for oxygen evolution reaction of water splitting.

    PubMed

    Cheng, Yi; Liu, Chang; Cheng, Hui-Ming; Jiang, San Ping

    2014-07-01

    Oxygen evaluation reaction (OER) is the most important reaction in hydrogen production from water splitting. Here we developed metal-carbon nanotubes (M-CNTs) hybrids with high metal oxide catalyst loading synthesized by arc-discharge and chemical vapor deposition (CVD) methods as electrocatalysts for OER in alkaline solutions. The M-CNTs hybrids produced by arc-discharge (M-CNTs-Arc) and CVD (M-CNTs-CVD) exhibit a core-shell-like structure, in which metal nanoparticles (NPs) encapsulated by graphite shells are connected by carbon nanotubes (CNTs), forming M-CNTs network hybrids. M-CNTs-Arc has NiCo0.16Fe0.34 metal core and shows very high activity and superior stability for OER, achieving 100 A g(-1) at an overpotential (η) of 0.29 V and 500 A g(-1) at η = 0.37 V in 1 M KOH solution. This is probably the highest activity reported for OER in alkaline solutions. The reaction follows the first-order kinetics with respect to OH(-) concentration and Tafel slope of 34 mV dec(-1). The results demonstrate a highly efficient, scalable, and low-cost one-step synthesis method for developing highly active and stable catalysts for electrochemical water splitting in alkaline solutions. PMID:24927372

  13. One-Pot Isomerization–Cross Metathesis–Reduction (ICMR) Synthesis of Lipophilic Tetrapeptides

    PubMed Central

    2015-01-01

    An efficient, versatile and rapid method toward homologue series of lipophilic tetrapeptide derivatives (herein, the opioid peptides H-TIPP-OH and H-DIPP-OH) is reported. High atom economy and a minimal number of synthetic steps resulted from a one-pot tandem isomerization-cross metathesis-reduction sequence (ICMR), applicable both in solution and solid phase methodology. The broadly applicable synthesis proceeds with short reaction times and simple work-up, as illustrated in this work for alkylated opioid tetrapeptides. PMID:24906051

  14. One-pot facile green synthesis of biocidal silver nanoparticles

    NASA Astrophysics Data System (ADS)

    Nudrat Hazarika, Shabiha; Gupta, Kuldeep; Shamin, Khan Naseem Ahmed Mohammed; Bhardwaj, Pushpender; Boruah, Ratan; Yadav, Kamlesh K.; Naglot, Ashok; Deb, P.; Mandal, M.; Doley, Robin; Veer, Vijay; Baruah, Indra; Namsa, Nima D.

    2016-07-01

    The plant root extract mediated green synthesis method produces monodispersed spherical shape silver nanoparticles (AgNPs) with a size range of 15–30 nm as analyzed by atomic force and transmission electron microscopy. The material showed potent antibacterial and antifungal properties. Synthesized AgNPs display a characteristic surface plasmon resonance peak at 420 nm in UV–Vis spectroscopy. X-ray diffractometer analysis revealed the crystalline and face-centered cubic geometry of in situ prepared AgNPs. Agar well diffusion and a colony forming unit assay demonstrated the potent biocidal activity of AgNPs against Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Klebsiella pneumoniae, Pseudomonas diminuta and Mycobacterium smegmatis. Intriguingly, the phytosynthesized AgNPs exhibited activity against pathogenic fungi, namely Trichophyton rubrum, Aspergillus versicolor and Candida albicans. Scanning electron microscopy observations indicated morphological changes in the bacterial cells incubated with silver nanoparticles. The genomic DNA isolated from the bacteria was incubated with an increasing concentration of AgNPs and the replication fidelity of 16S rDNA was observed by performing 18 and 35 cycles PCR. The replication efficiency of small (600 bp) and large (1500 bp) DNA fragments in the presence of AgNPs were compromised in a dose-dependent manner. The results suggest that the Thalictrum foliolosum root extract mediated synthesis of AgNPs could be used as a promising antimicrobial agent against clinical pathogens.

  15. One-pot facile green synthesis of biocidal silver nanoparticles

    NASA Astrophysics Data System (ADS)

    Nudrat Hazarika, Shabiha; Gupta, Kuldeep; Shamin, Khan Naseem Ahmed Mohammed; Bhardwaj, Pushpender; Boruah, Ratan; Yadav, Kamlesh K.; Naglot, Ashok; Deb, P.; Mandal, M.; Doley, Robin; Veer, Vijay; Baruah, Indra; Namsa, Nima D.

    2016-07-01

    The plant root extract mediated green synthesis method produces monodispersed spherical shape silver nanoparticles (AgNPs) with a size range of 15-30 nm as analyzed by atomic force and transmission electron microscopy. The material showed potent antibacterial and antifungal properties. Synthesized AgNPs display a characteristic surface plasmon resonance peak at 420 nm in UV-Vis spectroscopy. X-ray diffractometer analysis revealed the crystalline and face-centered cubic geometry of in situ prepared AgNPs. Agar well diffusion and a colony forming unit assay demonstrated the potent biocidal activity of AgNPs against Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Klebsiella pneumoniae, Pseudomonas diminuta and Mycobacterium smegmatis. Intriguingly, the phytosynthesized AgNPs exhibited activity against pathogenic fungi, namely Trichophyton rubrum, Aspergillus versicolor and Candida albicans. Scanning electron microscopy observations indicated morphological changes in the bacterial cells incubated with silver nanoparticles. The genomic DNA isolated from the bacteria was incubated with an increasing concentration of AgNPs and the replication fidelity of 16S rDNA was observed by performing 18 and 35 cycles PCR. The replication efficiency of small (600 bp) and large (1500 bp) DNA fragments in the presence of AgNPs were compromised in a dose-dependent manner. The results suggest that the Thalictrum foliolosum root extract mediated synthesis of AgNPs could be used as a promising antimicrobial agent against clinical pathogens.

  16. One-pot enzymatic synthesis of merochlorin A and B.

    PubMed

    Teufel, Robin; Kaysser, Leonard; Villaume, Matthew T; Diethelm, Stefan; Carbullido, Mary K; Baran, Phil S; Moore, Bradley S

    2014-10-01

    The polycycles merochlorin A and B are complex halogenated meroterpenoid natural products with significant antibacterial activities and are produced by the marine bacterium Streptomyces sp. strain CNH-189. Heterologously produced enzymes and chemical synthesis are employed herein to fully reconstitute the merochlorin biosynthesis in vitro. The interplay of a dedicated type III polyketide synthase, a prenyl diphosphate synthase, and an aromatic prenyltransferase allow formation of a highly unusual aromatic polyketide-terpene hybrid intermediate which features an unprecedented branched sesquiterpene moiety from isosesquilavandulyl diphosphate. As supported by in vivo experiments, this precursor is furthermore chlorinated and cyclized to merochlorin A and isomeric merochlorin B by a single vanadium-dependent haloperoxidase, thus completing the remarkably efficient pathway.

  17. Simple one-pot synthesis of Rh-Fe3O4 heterodimer nanocrystals and their applications to a magnetically recyclable catalyst for efficient and selective reduction of nitroarenes and alkenes.

    PubMed

    Jang, Youngjin; Kim, Seyoung; Jun, Samuel Woojoo; Kim, Byung Hyo; Hwang, Sunhwan; Song, In Kyu; Kim, B Moon; Hyeon, Taeghwan

    2011-03-28

    A simple synthesis of Rh-Fe(3)O(4) heterodimer nanocrystals was achieved by controlled one-pot thermolysis. The nanocrystals exhibited excellent activities for the selective reduction of nitroarenes and alkenes. Furthermore the nanocrystal catalyst could be easily separated by a magnet, and recycled eight times without losing the catalytic activity.

  18. Precise Tuning of Facile One-Pot Gelatin Methacryloyl (GelMA) Synthesis

    PubMed Central

    Shirahama, Hitomi; Lee, Bae Hoon; Tan, Lay Poh; Cho, Nam-Joon

    2016-01-01

    Gelatin-methacryloyl (GelMA) is one of the most commonly used photopolymerizable biomaterials in bio-applications. However, GelMA synthesis remains suboptimal, as its reaction parameters have not been fully investigated. The goal of this study is to establish an optimal route for effective and controllable GelMA synthesis by systematically examining reaction parameters including carbonate-bicarbonate (CB) buffer molarity, initial pH adjustment, MAA concentration, gelatin concentration, reaction temperature, and reaction time. We employed several analytical techniques in order to determine the degree of substitution (DS) and conducted detailed structural analysis of the synthesized polymer. The results enabled us to optimize GelMA synthesis, showing the optimal conditions to balance the deprotonation of amino groups with minimizing MAA hydrolysis, which led to nearly complete substitution. The optimized conditions (low feed ratio of MAA to gelatin (0.1 mL/g), 0.25 M CB buffer at pH 9, and a gelatin concentration of 10–20%) enable a simplified reaction scheme that produces GelMA with high substitution with just one-step addition of MAA in one pot. Looking forward, these optimal conditions not only enable facile one-pot GelMA synthesis but can also guide researchers to explore the efficient, high methacrylation of other biomacromolecules. PMID:27503340

  19. Precise Tuning of Facile One-Pot Gelatin Methacryloyl (GelMA) Synthesis

    NASA Astrophysics Data System (ADS)

    Shirahama, Hitomi; Lee, Bae Hoon; Tan, Lay Poh; Cho, Nam-Joon

    2016-08-01

    Gelatin-methacryloyl (GelMA) is one of the most commonly used photopolymerizable biomaterials in bio-applications. However, GelMA synthesis remains suboptimal, as its reaction parameters have not been fully investigated. The goal of this study is to establish an optimal route for effective and controllable GelMA synthesis by systematically examining reaction parameters including carbonate-bicarbonate (CB) buffer molarity, initial pH adjustment, MAA concentration, gelatin concentration, reaction temperature, and reaction time. We employed several analytical techniques in order to determine the degree of substitution (DS) and conducted detailed structural analysis of the synthesized polymer. The results enabled us to optimize GelMA synthesis, showing the optimal conditions to balance the deprotonation of amino groups with minimizing MAA hydrolysis, which led to nearly complete substitution. The optimized conditions (low feed ratio of MAA to gelatin (0.1 mL/g), 0.25 M CB buffer at pH 9, and a gelatin concentration of 10–20%) enable a simplified reaction scheme that produces GelMA with high substitution with just one-step addition of MAA in one pot. Looking forward, these optimal conditions not only enable facile one-pot GelMA synthesis but can also guide researchers to explore the efficient, high methacrylation of other biomacromolecules.

  20. Precise Tuning of Facile One-Pot Gelatin Methacryloyl (GelMA) Synthesis.

    PubMed

    Shirahama, Hitomi; Lee, Bae Hoon; Tan, Lay Poh; Cho, Nam-Joon

    2016-08-09

    Gelatin-methacryloyl (GelMA) is one of the most commonly used photopolymerizable biomaterials in bio-applications. However, GelMA synthesis remains suboptimal, as its reaction parameters have not been fully investigated. The goal of this study is to establish an optimal route for effective and controllable GelMA synthesis by systematically examining reaction parameters including carbonate-bicarbonate (CB) buffer molarity, initial pH adjustment, MAA concentration, gelatin concentration, reaction temperature, and reaction time. We employed several analytical techniques in order to determine the degree of substitution (DS) and conducted detailed structural analysis of the synthesized polymer. The results enabled us to optimize GelMA synthesis, showing the optimal conditions to balance the deprotonation of amino groups with minimizing MAA hydrolysis, which led to nearly complete substitution. The optimized conditions (low feed ratio of MAA to gelatin (0.1 mL/g), 0.25 M CB buffer at pH 9, and a gelatin concentration of 10-20%) enable a simplified reaction scheme that produces GelMA with high substitution with just one-step addition of MAA in one pot. Looking forward, these optimal conditions not only enable facile one-pot GelMA synthesis but can also guide researchers to explore the efficient, high methacrylation of other biomacromolecules.

  1. Precise Tuning of Facile One-Pot Gelatin Methacryloyl (GelMA) Synthesis.

    PubMed

    Shirahama, Hitomi; Lee, Bae Hoon; Tan, Lay Poh; Cho, Nam-Joon

    2016-01-01

    Gelatin-methacryloyl (GelMA) is one of the most commonly used photopolymerizable biomaterials in bio-applications. However, GelMA synthesis remains suboptimal, as its reaction parameters have not been fully investigated. The goal of this study is to establish an optimal route for effective and controllable GelMA synthesis by systematically examining reaction parameters including carbonate-bicarbonate (CB) buffer molarity, initial pH adjustment, MAA concentration, gelatin concentration, reaction temperature, and reaction time. We employed several analytical techniques in order to determine the degree of substitution (DS) and conducted detailed structural analysis of the synthesized polymer. The results enabled us to optimize GelMA synthesis, showing the optimal conditions to balance the deprotonation of amino groups with minimizing MAA hydrolysis, which led to nearly complete substitution. The optimized conditions (low feed ratio of MAA to gelatin (0.1 mL/g), 0.25 M CB buffer at pH 9, and a gelatin concentration of 10-20%) enable a simplified reaction scheme that produces GelMA with high substitution with just one-step addition of MAA in one pot. Looking forward, these optimal conditions not only enable facile one-pot GelMA synthesis but can also guide researchers to explore the efficient, high methacrylation of other biomacromolecules. PMID:27503340

  2. Synthesis of manganese incorporated hierarchical mesoporous silica nanosphere with fibrous morphology by facile one-pot approach for efficient catalytic ozonation.

    PubMed

    Afzal, Shahzad; Quan, Xie; Chen, Shuo; Wang, Jing; Muhammad, Dost

    2016-11-15

    Manganese incorporated fibrous silica nanosphere (MnOx-0.013/KCC-1) was synthesized by one step hydrothermal method for the first time and its catalytic activity for ozonation of oxalic acid was studied. For comparison, manganese loaded MCM-41 (MnOx-0.013/MCM-41) was prepared by impregnation method. Various characterizations showed that the morphological, structural and textural properties of MnOx-0.013/KCC-1 were well preserved. Ozonation and catalytic ozonation by MnOx-0.013/KCC-1 and MnOx-0.013/MCM-41 led to 4, 85 and 60% reduction in TOC respectively. Furthermore, 0.05 and 1.2mgL(-1) leaching of Mn was detected from MnOx-0.013/KCC-1 and MnOx-0.013/MCM-41, which are approximately 2.0 and 42.0% of the total Mn present in MnOx-0.013/KCC-1 and MnOx-0.013/MCM-41 respectively. The high catalytic activity was attributed to the generation of hydroxyl radical. Surface hydroxyl groups investigated by using phosphates and ATR-FTIR were believed to be the active sites. Our proposed method of synthesis can be generalized for the synthesis of other metal oxides incorporated fibrous silica for environmental catalysis and other catalytic reactions.

  3. Synthesis of manganese incorporated hierarchical mesoporous silica nanosphere with fibrous morphology by facile one-pot approach for efficient catalytic ozonation.

    PubMed

    Afzal, Shahzad; Quan, Xie; Chen, Shuo; Wang, Jing; Muhammad, Dost

    2016-11-15

    Manganese incorporated fibrous silica nanosphere (MnOx-0.013/KCC-1) was synthesized by one step hydrothermal method for the first time and its catalytic activity for ozonation of oxalic acid was studied. For comparison, manganese loaded MCM-41 (MnOx-0.013/MCM-41) was prepared by impregnation method. Various characterizations showed that the morphological, structural and textural properties of MnOx-0.013/KCC-1 were well preserved. Ozonation and catalytic ozonation by MnOx-0.013/KCC-1 and MnOx-0.013/MCM-41 led to 4, 85 and 60% reduction in TOC respectively. Furthermore, 0.05 and 1.2mgL(-1) leaching of Mn was detected from MnOx-0.013/KCC-1 and MnOx-0.013/MCM-41, which are approximately 2.0 and 42.0% of the total Mn present in MnOx-0.013/KCC-1 and MnOx-0.013/MCM-41 respectively. The high catalytic activity was attributed to the generation of hydroxyl radical. Surface hydroxyl groups investigated by using phosphates and ATR-FTIR were believed to be the active sites. Our proposed method of synthesis can be generalized for the synthesis of other metal oxides incorporated fibrous silica for environmental catalysis and other catalytic reactions. PMID:27434734

  4. Efficient one-pot synthesis of hierarchical flower-like α-Fe2O3 hollow spheres with excellent adsorption performance for water treatment

    NASA Astrophysics Data System (ADS)

    Zhu, Daozheng; Zhang, Jian; Song, Jiming; Wang, Haisheng; Yu, Zheng; Shen, Yuhua; Xie, Anjian

    2013-11-01

    A simple one-step method has been developed for the controllable synthesis of hierarchical flower-like α-Fe2O3 hollow spheres in a glycerol-ethanol system. It is found that the volume ratio of glycerol/ethanol and reaction time have a significant effect on the morphology of the products. The growth process of α-Fe2O3 hollow spheres has been investigated and a possible mechanism is proposed. The α-Fe2O3 hollow spheres have a high surface area of 98 m2 g-1 and a total pore volume of 0.32 cm3 g-1, which exhibit outstanding water treatment performance with high removal capacities toward organic dyes and heavy metal ions. The as-obtained products may have potential applications in water treatment and other related micro- or nanoscale devices.

  5. One-pot multienzyme (OPME) systems for chemoenzymatic synthesis of carbohydrates.

    PubMed

    Yu, Hai; Chen, Xi

    2016-03-14

    Glycosyltransferase-catalyzed enzymatic and chemoenzymatic syntheses are powerful approaches for the production of oligosaccharides, polysaccharides, glycoconjugates, and their derivatives. Enzymes involved in the biosynthesis of sugar nucleotide donors can be combined with glycosyltransferases in one pot for efficient production of the target glycans from simple monosaccharides and acceptors. The identification of enzymes involved in the salvage pathway of sugar nucleotide generation has greatly facilitated the development of simplified and efficient one-pot multienzyme (OPME) systems for synthesizing major glycan epitopes in mammalian glycomes. The applications of OPME methods are steadily gaining popularity mainly due to the increasing availability of wild-type and engineered enzymes. Substrate promiscuity of these enzymes and their mutants allows OPME synthesis of carbohydrates with naturally occurring post-glycosylational modifications (PGMs) and their non-natural derivatives using modified monosaccharides as precursors. The OPME systems can be applied in sequence for synthesizing complex carbohydrates. The sequence of the sequential OPME processes, the glycosyltransferase used, and the substrate specificities of the glycosyltransferases define the structures of the products. The OPME and sequential OPME strategies can be extended to diverse glycans in other glycomes when suitable enzymes with substrate promiscuity become available. This Perspective summarizes the work of the authors and collaborators on the development of glycosyltransferase-based OPME systems for carbohydrate synthesis. Future directions are also discussed.

  6. One-pot synthesis of nitrogen and sulfur co-doped graphene as efficient metal-free electrocatalysts for the oxygen reduction reaction.

    PubMed

    Wang, Xin; Wang, Jie; Wang, Deli; Dou, Shuo; Ma, Zhaoling; Wu, Jianghong; Tao, Li; Shen, Anli; Ouyang, Canbin; Liu, Qiuhong; Wang, Shuangyin

    2014-05-14

    Novel N, S co-doped graphene (NSG) was prepared by annealing graphene oxide with thiourea as the single N and S precursor. The NSG electrodes, as efficient metal-free electrocatalysts, show a direct four-electron reaction pathway, high onset potential, high current density and high stability for the oxygen reduction reaction.

  7. One pot aqueous synthesis of nanoporous Au85Pt15 material with surface bound Pt islands: an efficient methanol tolerant ORR catalyst

    NASA Astrophysics Data System (ADS)

    Anandha Ganesh, P.; Jeyakumar, D.

    2014-10-01

    For the first time, we are reporting the synthesis of Au100-xPtx nanoporous materials in the size range of 7-10 nm through the galvanic replacement of Ag by Pt from Au100-xAg2x spherical nano-alloys (x = 20, 15, 10 and 5) in an aqueous medium. The galvanic replacement reaction follows the `Volmer-Weber' growth mode, resulting in the formation of surface bound platinum islands on a nanoporous gold surface. The high angle annular dark field image and low angle X-ray diffraction studies confirm the presence of nanoporous Au100-xPtx NPs. The electrochemical studies using the Au85Pt15/C catalyst show excellent methanol tolerance behaviour and better performance towards oxygen reduction reaction (ORR) in terms of high mass activity, mass-specific activity and figure of merit (FOM) when compared to HiSPEC Pt/C commercial catalyst. Preliminary studies on a full cell using nanoporous Au85Pt15/C (loading 1.0 mg cm-2) as the cathode material and Pt-Ru/C (loading: 0.5 mg cm-2) as the anode material performed better (38 mW cm-2) than the HiSPEC Pt/C cathode material (16 mW cm-2).For the first time, we are reporting the synthesis of Au100-xPtx nanoporous materials in the size range of 7-10 nm through the galvanic replacement of Ag by Pt from Au100-xAg2x spherical nano-alloys (x = 20, 15, 10 and 5) in an aqueous medium. The galvanic replacement reaction follows the `Volmer-Weber' growth mode, resulting in the formation of surface bound platinum islands on a nanoporous gold surface. The high angle annular dark field image and low angle X-ray diffraction studies confirm the presence of nanoporous Au100-xPtx NPs. The electrochemical studies using the Au85Pt15/C catalyst show excellent methanol tolerance behaviour and better performance towards oxygen reduction reaction (ORR) in terms of high mass activity, mass-specific activity and figure of merit (FOM) when compared to HiSPEC Pt/C commercial catalyst. Preliminary studies on a full cell using nanoporous Au85Pt15/C (loading 1.0 mg

  8. Combined Pd/C and Montmorillonite Catalysis for One-Pot Synthesis of Benzimidazoles.

    PubMed

    Weires, Nicholas A; Boster, Jared; Magolan, Jakob

    2012-11-01

    A series of nineteen benzimidazoles are prepared from ortho-nitroanilines via one-pot transfer hydrogenation, condensation, and dehydrogenation enabled by the concurrent use of two heterogeneous catalysts: montmorillonite-K10 and Pd/C. This strategy is further employed to accomplish a five-step, three-component synthesis of an antifungal benzimidazoquinazoline using a simple one-pot procedure. PMID:23525858

  9. Combined Pd/C and Montmorillonite Catalysis for One-Pot Synthesis of Benzimidazoles

    PubMed Central

    Weires, Nicholas A.; Boster, Jared; Magolan, Jakob

    2013-01-01

    A series of nineteen benzimidazoles are prepared from ortho-nitroanilines via one-pot transfer hydrogenation, condensation, and dehydrogenation enabled by the concurrent use of two heterogeneous catalysts: montmorillonite-K10 and Pd/C. This strategy is further employed to accomplish a five-step, three-component synthesis of an antifungal benzimidazoquinazoline using a simple one-pot procedure. PMID:23525858

  10. One-pot in situ redox synthesis of hexacyanoferrate/conductive polymer hybrids as lithium-ion battery cathodes.

    PubMed

    Wong, Min Hao; Zhang, Zixuan; Yang, Xianfeng; Chen, Xiaojun; Ying, Jackie Y

    2015-09-14

    An efficient and adaptable method is demonstrated for the synthesis of lithium hexacyanoferrate/conductive polymer hybrids for Li-ion battery cathodes. The hybrids were synthesized via a one-pot method, involving a redox-coupled reaction between pyrrole monomers and the Li3Fe(CN)6 precursor. The hybrids showed much better cyclability relative to reported Prussian Blue (PB) analogs.

  11. One-pot synthesis of S-alkyl dithiocarbamates via the reaction of N-tosylhydrazones, carbon disulfide and amines.

    PubMed

    Sha, Qiang; Wei, Yun-Yang

    2013-09-14

    A new, convenient and efficient transition metal-free synthesis of S-alkyl dithiocarbamates through one-pot reaction of N-tosylhydrazones, carbon disulfide and amines is reported. Tosylhydrazones derived from various aromatic and aliphatic ketones or aldehydes were tested and gave dithiocarbamates in good to excellent yields. The tosylhydrazones can be generated in situ without isolation, which provides a simpler one-pot method to synthesize dithiocarbamates via the reaction of carbonyl compounds, carbon disulfide and amines in the presence of 4-methylbenzenesulfonohydrazide. PMID:23863979

  12. Facile One-Pot Polyol Method for the Synthesis of Uniform Size Silver Nanowires.

    PubMed

    Kaili, Zhang; Yongguo, Du; Shimin, Chen

    2016-01-01

    This study reports the development of a facile and efficient one-pot polyol method for the synthesis of silver nanowires. The seed and growth of silver nanowires under different reaction conditions were characterized and measured. The pertinent variables such as temperature, time, concentration and capping agent were investigated. Moreover, the effect of seeding at two different stages-initial stage and secondary stage-was studied and discussed on the size control of silver nanowires. In particular, silver nanowires with diameter less than 40 nm and length over 25 µm in a narrow distribution, was obtained through a novel method in which reaction flask was placed in a low-temperature bath after seeding for some time in the high-temperature bath. This approach may be useful for the fabrication of uniform, large aspect ratio silver nanowires for optoelectronic applications. PMID:27398477

  13. Facile One-Pot Polyol Method for the Synthesis of Uniform Size Silver Nanowires.

    PubMed

    Kaili, Zhang; Yongguo, Du; Shimin, Chen

    2016-01-01

    This study reports the development of a facile and efficient one-pot polyol method for the synthesis of silver nanowires. The seed and growth of silver nanowires under different reaction conditions were characterized and measured. The pertinent variables such as temperature, time, concentration and capping agent were investigated. Moreover, the effect of seeding at two different stages-initial stage and secondary stage-was studied and discussed on the size control of silver nanowires. In particular, silver nanowires with diameter less than 40 nm and length over 25 µm in a narrow distribution, was obtained through a novel method in which reaction flask was placed in a low-temperature bath after seeding for some time in the high-temperature bath. This approach may be useful for the fabrication of uniform, large aspect ratio silver nanowires for optoelectronic applications.

  14. Tuneable light-emitting carbon-dot/polymer flexible films prepared through one-pot synthesis.

    PubMed

    Bhunia, Susanta Kumar; Nandi, Sukhendu; Shikler, Rafi; Jelinek, Raz

    2016-02-14

    Development of efficient, inexpensive, and environmentally-friendly light emitters, particularly devices that produce white light, have drawn intense interest due to diverse applications in the lighting industry, photonics, solar energy, and others. We present a simple strategy for the fabrication of flexible transparent films exhibiting tuneable light emission through one-pot synthesis of polymer matrixes with embedded carbon dots assembled in situ. Importantly, different luminescence colours were produced simply by preparing C-dot/polymer films using carbon precursors that yielded C-dots exhibiting distinct fluorescence emission profiles. Furthermore, mixtures of C-dot precursors could be also employed for fabricating films exhibiting different colours. In particular, we successfully produced films emitting white light with attractive properties (i.e."warm" white light with a high colour rendering index) - a highly sought after goal in optical technologies. PMID:26791813

  15. Tuneable light-emitting carbon-dot/polymer flexible films prepared through one-pot synthesis

    NASA Astrophysics Data System (ADS)

    Bhunia, Susanta Kumar; Nandi, Sukhendu; Shikler, Rafi; Jelinek, Raz

    2016-02-01

    Development of efficient, inexpensive, and environmentally-friendly light emitters, particularly devices that produce white light, have drawn intense interest due to diverse applications in the lighting industry, photonics, solar energy, and others. We present a simple strategy for the fabrication of flexible transparent films exhibiting tuneable light emission through one-pot synthesis of polymer matrixes with embedded carbon dots assembled in situ. Importantly, different luminescence colours were produced simply by preparing C-dot/polymer films using carbon precursors that yielded C-dots exhibiting distinct fluorescence emission profiles. Furthermore, mixtures of C-dot precursors could be also employed for fabricating films exhibiting different colours. In particular, we successfully produced films emitting white light with attractive properties (i.e. ``warm'' white light with a high colour rendering index) - a highly sought after goal in optical technologies.Development of efficient, inexpensive, and environmentally-friendly light emitters, particularly devices that produce white light, have drawn intense interest due to diverse applications in the lighting industry, photonics, solar energy, and others. We present a simple strategy for the fabrication of flexible transparent films exhibiting tuneable light emission through one-pot synthesis of polymer matrixes with embedded carbon dots assembled in situ. Importantly, different luminescence colours were produced simply by preparing C-dot/polymer films using carbon precursors that yielded C-dots exhibiting distinct fluorescence emission profiles. Furthermore, mixtures of C-dot precursors could be also employed for fabricating films exhibiting different colours. In particular, we successfully produced films emitting white light with attractive properties (i.e. ``warm'' white light with a high colour rendering index) - a highly sought after goal in optical technologies. Electronic supplementary information (ESI

  16. Unsymmetrical Aryl(2,4,6-trimethoxyphenyl)iodonium Salts: One-Pot Synthesis, Scope, Stability, and Synthetic Studies.

    PubMed

    Seidl, Thomas L; Sundalam, Sunil K; McCullough, Brennen; Stuart, David R

    2016-03-01

    Diaryliodonium salts have recently attracted significant attention as metal-free-arylation reagents in organic synthesis, and efficient access to these salts is critical for advancement of their use in reaction discovery and development. The trimethoxybenzene-derived auxiliary is a promising component of unsymmetrical variants, yet access remains limited. Here, a one-pot synthesis of aryl(2,4,6-trimethoxyphenyl)iodonium salts from aryl iodides, m-CPBA, p-toluenesulfonic acid, and trimethoxybenzene is described. Optimization of the reaction conditions for this one-pot synthesis was enabled by the method of multivariate analysis. The reaction is fast (<1 h), provides a high yield of product (>85% average), and has broad substrate scope (>25 examples) including elaborate aryl iodides. The utility of these reagents is demonstrated in moderate to high yielding arylation reactions with C-, N-, O-, and S-nucleophiles including the synthesis of a liquid crystal molecule.

  17. Facile one-pot synthesis of unsymmetrical ureas, carbamates, and thiocarbamates from Cbz-protected amines.

    PubMed

    Kim, Hee-Kwon; Lee, Anna

    2016-07-26

    A novel one-pot synthesis of unsymmetrical ureas, carbamates and thiocarbamates from Cbz-protected amines has been developed. In the presence of 2-chloropyridine and trifluoromethanesulfonyl anhydride, isocyanates are generated in situ, which facilitate rapid reaction with amines, alcohols, and thiols to afford the corresponding ureas, carbamates and thiocarbamates in high yields. PMID:27406041

  18. Dienamine and Friedel-Crafts one-pot synthesis, and antitumor evaluation of diheteroarylalkanals.

    PubMed

    Frías, María; Padrón, José M; Alemán, José

    2015-05-26

    An asymmetric synthesis of diheteroarylalkanals through one-pot dienamine and Friedel-Crafts reaction is presented. The reaction tolerates a large variety of substituents at different positions of the starting aldehyde and also in the indole nucleophile, and a range of diheterocyclic alkanals can be achieved. Furthermore, we have studied the antiproliferative activity of these new compounds in representative cancer tumor cell lines.

  19. Photocatalytic One-Pot Synthesis of Homoallyl Ketones via a Norrish Type I Reaction of Cyclopentanones.

    PubMed

    Okada, Megumi; Yamada, Keiichi; Fukuyama, Takahide; Ravelli, Davide; Fagnoni, Maurizio; Ryu, Ilhyong

    2015-09-18

    A photocatalytic synthesis of homoallyl ketones was achieved via a one-pot procedure starting from a Norrish Type I reaction of cyclopentanones, followed by a decatungstate-catalyzed hydroacylation of electron-deficient olefins by the resulting 4-pentenals. The site-selective formyl H-abstraction in the second step can be explained by radical polar effects in the transition state.

  20. "One-pot" synthesis of amidoxime via Pd-catalyzed cyanation and amidoximation.

    PubMed

    Yang, Chu-Ting; Han, Jun; Liu, Jun; Gu, Mei; Li, Yi; Wen, Jun; Yu, Hai-Zhu; Hu, Sheng; Wang, Xiaolin

    2015-03-01

    A novel "one-pot" reaction was developed for the synthesis of aryl or heteroaryl-substituted amidoxime compounds containing various functional groups. Fluorescence titration experiments coupled with theoretical analysis revealed that the steric hindrance and electronic effects of substituents influence the binding ability of the amidoxime compounds to uranyl ions.

  1. One-pot synthesis, optical property and self-assembly of monodisperse silver nanospheres

    SciTech Connect

    Tang Aiwei; Qu Shengchun; Hou Yanbing; Teng Feng; Wang Yongsheng; Wang Zhanguo

    2011-08-15

    High-quality spherical silver (Ag) nanocrystals have been synthesized by using a one-pot approach, in which pre-synthesis of organometallic precursors is not required. This reaction involves the thermolysis of a mixed solution of silver acetate and n-dodecanethiol in a non-coordinating organic solvent. The size of the as-obtained Ag nanospheres can be controlled by adjusting the reaction time, reaction temperature and the amount of silver acetate added. The growth and nucleation process of the resultant Ag nanospheres have been studied by employing UV-vis absorption spectra and transmission electron microscopy (TEM) images. Furthermore, these Ag nanospheres have good self-assembly behaviors, and they are easily self-assembled into two- or three-dimensional superlattice structures due to the bundling and interdigitation of thiolate molecules adsorbed on Ag nanospheres. This one-pot synthetic procedure is simple and highly reproducible, which may be extended to prepare other noble-metal nanocrystals. - Graphical abstract: Different sized and monodisperse silver nanospheres were prepared using a one-pot approach with no pre-synthesis of organometallic precursors, and the silver nanospheres can self-assemble into highly ordered superlattices. Highlights: > Monodisperse silver nanospheres have been synthesized by a one-pot approach. > The synthetic method does not need pre-synthesis of organometallic precursors. > The silver nanospheres can self-assemble into highly ordered superlattices. > This synthetic method can be extended to prepare other metal nanocrystals.

  2. Nanotexaphyrin: One-Pot Synthesis of a Manganese Texaphyrin-Phospholipid Nanoparticle for Magnetic Resonance Imaging.

    PubMed

    Keca, Joseph M; Chen, Juan; Overchuk, Marta; Muhanna, Nidal; MacLaughlin, Christina M; Jin, Cheng S; Foltz, Warren D; Irish, Jonathan C; Zheng, Gang

    2016-05-17

    The discovery and synthesis of novel multifunctional organic building blocks for nanoparticles is challenging. Texaphyrin macrocycles are capable and multifunctional chelators. However, they remain elusive as building blocks for nanoparticles because of the difficulty associated with synthesis of texaphyrin constructs capable of self-assembly. A novel manganese (Mn)-texaphyrin-phospholipid building block is described, along with its one-pot synthesis and self-assembly into a Mn-nanotexaphyrin. This nanoparticle possesses strong resilience to manganese dissociation, structural stability, in vivo bio-safety, and structure-dependent T1 and T2 relaxivities. Magnetic resonance imaging (MRI) contrast enhanced visualization of lymphatic drainage is demonstrated with respect to proximal lymph nodes on the head and neck VX-2 tumors of a rabbit. Synthesis of 17 additional metallo-texaphyrin building blocks suggests that this novel one-pot synthetic procedure for nanotexaphyrins may lead to a wide range of applications in the field of nanomedicines. PMID:27071806

  3. Nanotexaphyrin: One-Pot Synthesis of a Manganese Texaphyrin-Phospholipid Nanoparticle for Magnetic Resonance Imaging.

    PubMed

    Keca, Joseph M; Chen, Juan; Overchuk, Marta; Muhanna, Nidal; MacLaughlin, Christina M; Jin, Cheng S; Foltz, Warren D; Irish, Jonathan C; Zheng, Gang

    2016-05-17

    The discovery and synthesis of novel multifunctional organic building blocks for nanoparticles is challenging. Texaphyrin macrocycles are capable and multifunctional chelators. However, they remain elusive as building blocks for nanoparticles because of the difficulty associated with synthesis of texaphyrin constructs capable of self-assembly. A novel manganese (Mn)-texaphyrin-phospholipid building block is described, along with its one-pot synthesis and self-assembly into a Mn-nanotexaphyrin. This nanoparticle possesses strong resilience to manganese dissociation, structural stability, in vivo bio-safety, and structure-dependent T1 and T2 relaxivities. Magnetic resonance imaging (MRI) contrast enhanced visualization of lymphatic drainage is demonstrated with respect to proximal lymph nodes on the head and neck VX-2 tumors of a rabbit. Synthesis of 17 additional metallo-texaphyrin building blocks suggests that this novel one-pot synthetic procedure for nanotexaphyrins may lead to a wide range of applications in the field of nanomedicines.

  4. A one-pot synthesis of reduced graphene oxide-Cu₂S quantum dot hybrids for optoelectronic devices.

    PubMed

    Su, Yanjie; Lu, Xiaonan; Xie, Minmin; Geng, Huijuan; Wei, Hao; Yang, Zhi; Zhang, Yafei

    2013-10-01

    We demonstrate a facile one-pot approach for the synthesis of reduced graphene oxide (rGO)-cuprous sulfide quantum dot (Cu₂S QD) hybrids, wherein the reduction of GO and the growth of Cu₂S QDs on graphene occur simultaneously. The as-synthesized rGO-Cu₂S QD hybrids exhibit an excellent photoelectric response and efficient electron transfer from the Cu₂S QDs to the rGO sheets.

  5. One-Pot Synthesis of Benzothiazole-Tethered Chromanones/Coumarins via Claisen Rearrangement Using the Solid State Melt Reaction.

    PubMed

    Bakthadoss, Manickam; Selvakumar, Raman

    2016-04-15

    A novel protocol has been successfully established for the efficient synthesis of benzothiazole-tethered chromanone/coumarin scaffolds via Claisen rearrangement using a solid state melt reaction in a one-pot manner. Benzothiazole formation and Claisen rearrangement involve the cleavage of S-S and C-O bonds and formation of C-S, C═N, and C-C bonds in a single operation without using a catalyst or solvent. PMID:26991666

  6. The use of calcium carbide in one-pot synthesis of symmetric diaryl ethynes.

    PubMed

    Zhang, Weiwei; Wu, Huayue; Liu, Zhiqing; Zhong, Ping; Zhang, Lin; Huang, Xiaobo; Cheng, Jiang

    2006-12-14

    An efficient Pd-catalyzed copper and amine free coupling reaction of acetylene and aryl bromides was achieved with calcium carbide as an acetylene source, using inorganic base and easily prepared, air-stable aminophosphine ligand in common organic solvents, providing symmetric diaryl ethynes in one-pot with yields ranged from moderate to excellent.

  7. Microwave-assisted one-pot synthesis of 1,6-anhydrosugars and orthogonally protected thioglycosides.

    PubMed

    Ko, Yen-Chun; Tsai, Cheng-Fang; Wang, Cheng-Chung; Dhurandhare, Vijay M; Hu, Pu-Ling; Su, Ting-Yang; Lico, Larry S; Zulueta, Medel Manuel L; Hung, Shang-Cheng

    2014-10-15

    Living organisms employ glycans as recognition elements because of their large structural information density. Well-defined sugar structures are needed to fully understand and take advantage of glycan functions, but sufficient quantities of these compounds cannot be readily obtained from natural sources and have to be synthesized. Among the bottlenecks in the chemical synthesis of complex glycans is the preparation of suitably protected monosaccharide building blocks. Thus, easy, rapid, and efficient methods for building-block acquisition are desirable. Herein, we describe routes directly starting from the free sugars toward notable monosaccharide derivatives through microwave-assisted one-pot synthesis. The procedure followed the in situ generation of per-O-trimethylsilylated monosaccharide intermediates, which provided 1,6-anhydrosugars or thioglycosides upon treatment with either trimethylsilyl trifluoromethanesulfonate or trimethyl(4-methylphenylthio)silane and ZnI2, respectively, under microwave irradiation. We successfully extended the methodology to regioselective protecting group installation and manipulation toward a number of thioglucosides and the glycosylation of persilylated derivatives, all of which were conducted in a single vessel. These developed approaches open the possibility for generating arrays of suitably protected building blocks for oligosaccharide assembly in a short period with minimal number of purification stages. PMID:25291402

  8. One-pot synthesis of thermoplastic mixed paramylon esters using trifluoroacetic anhydride.

    PubMed

    Shibakami, Motonari; Tsubouchi, Gen; Sohma, Mitsugu; Hayashi, Masahiro

    2015-03-30

    Mixed paramylon esters prepared from paramylon (a storage polysaccharide of Euglena), acetic acid, and a long-chain fatty acid by one-pot synthesis using trifluoroacetic anhydride as a promoter and solvent were shown to have thermoplasticity. Size exclusion chromatography indicated that the mixed paramylon esters had a weight average molecular weight of approximately 4.9-6.7×10(5). Thermal analysis showed that these esters were stable in terms of the glass transition temperature (>90°C) and 5% weight loss temperature (>320°C). The degree of substitution of the long alkyl chain group, a dominant factor determining thermoplasticity, was controlled by tuning the feed molar ratio of acetic acid and long-chain fatty acid to paramylon. These results implied that the one-pot synthesis is useful for preparing structurally-well defined thermoplastic mixed paramylon esters with high molecular weight.

  9. One-pot synthesis of thermoplastic mixed paramylon esters using trifluoroacetic anhydride.

    PubMed

    Shibakami, Motonari; Tsubouchi, Gen; Sohma, Mitsugu; Hayashi, Masahiro

    2015-03-30

    Mixed paramylon esters prepared from paramylon (a storage polysaccharide of Euglena), acetic acid, and a long-chain fatty acid by one-pot synthesis using trifluoroacetic anhydride as a promoter and solvent were shown to have thermoplasticity. Size exclusion chromatography indicated that the mixed paramylon esters had a weight average molecular weight of approximately 4.9-6.7×10(5). Thermal analysis showed that these esters were stable in terms of the glass transition temperature (>90°C) and 5% weight loss temperature (>320°C). The degree of substitution of the long alkyl chain group, a dominant factor determining thermoplasticity, was controlled by tuning the feed molar ratio of acetic acid and long-chain fatty acid to paramylon. These results implied that the one-pot synthesis is useful for preparing structurally-well defined thermoplastic mixed paramylon esters with high molecular weight. PMID:25563938

  10. One-pot synthesis, optical property and self-assembly of monodisperse silver nanospheres

    NASA Astrophysics Data System (ADS)

    Tang, Aiwei; Qu, Shengchun; Hou, Yanbing; Teng, Feng; Wang, Yongsheng; Wang, Zhanguo

    2011-08-01

    High-quality spherical silver (Ag) nanocrystals have been synthesized by using a one-pot approach, in which pre-synthesis of organometallic precursors is not required. This reaction involves the thermolysis of a mixed solution of silver acetate and n-dodecanethiol in a non-coordinating organic solvent. The size of the as-obtained Ag nanospheres can be controlled by adjusting the reaction time, reaction temperature and the amount of silver acetate added. The growth and nucleation process of the resultant Ag nanospheres have been studied by employing UV-vis absorption spectra and transmission electron microscopy (TEM) images. Furthermore, these Ag nanospheres have good self-assembly behaviors, and they are easily self-assembled into two- or three-dimensional superlattice structures due to the bundling and interdigitation of thiolate molecules adsorbed on Ag nanospheres. This one-pot synthetic procedure is simple and highly reproducible, which may be extended to prepare other noble-metal nanocrystals.

  11. Unexpected one-pot synthesis of highly conjugated pentacyclic diquinoid compounds.

    PubMed

    Coletti, Alessia; Lentini, Sara; Conte, Valeria; Floris, Barbara; Bortolini, Olga; Sforza, Fabio; Grepioni, Fabrizia; Galloni, Pierluca

    2012-08-17

    A new class of pentacyclic diquinoid compounds has been synthesized with a facile one-pot reaction of two molecules of 2-hydroxynaphthoquinone and 1-bromoalkanes in the presence of ferrocene. These molecules were isolated as enol tautomers that exhibit intramolecular hydrogen bond and extended electronic conjugation as proved by the intense absorption spectrum with a broad band between 400 and 600 nm. The spectroscopic and electrochemical characterization of this new class of compounds has been performed. One of the synthesized diquinoid derivatives showed a significant cytotoxicity with IC(50) values of 25-50 μM against Cisplatin-Resistant SKOV3 and colon carcinoma SW480 cell lines. The results of our study provide a valuable tool to a one-pot synthesis of highly conjugated polyquinones, analogous to important biological systems, with significant antitumoral activity. PMID:22834705

  12. Divergent synthesis of chiral heterocycles via sequencing of enantioselective three-component reactions and one-pot subsequent cyclization reactions.

    PubMed

    Tang, Min; Xing, Dong; Huang, Haoxi; Hu, Wenhao

    2015-07-01

    A highly efficient sequencing of catalytic asymmetric three-component reactions of alcohols, diazo compounds and aldimines/aldehydes with one-pot subsequent cyclization reactions was reported. The development of a robust and versatile Rh(ii)/Zr(iv)-BINOL co-catalytic system not only gives high diastereo- and enantioselective controls of the three-component reaction, but also shows excellent functionality tolerances that allow a wide range of functionalities to be pre-installed in each component and readily undergo one-pot subsequent cyclization reactions, thus providing rapid and diversity-oriented synthesis (DOS) of different types of chiral nitrogen- and/or oxygen-containing polyfunctional heterocycles. PMID:25864421

  13. One-pot Synthesis of Metal-Organic Frameworks with Encapsulated Target Molecules and Their Applications for Controlled Drug Delivery.

    PubMed

    Zheng, Haoquan; Zhang, Yuning; Liu, Leifeng; Wan, Wei; Guo, Peng; Nyström, Andreas M; Zou, Xiaodong

    2016-01-27

    Many medical and chemical applications require target molecules to be delivered in a controlled manner at precise locations. Metal-organic frameworks (MOFs) have high porosity, large surface area, and tunable functionality and are promising carriers for such purposes. Current approaches for incorporating target molecules are based on multistep postfunctionalization. Here, we report a novel approach that combines MOF synthesis and molecule encapsulation in a one-pot process. We demonstrate that large drug and dye molecules can be encapsulated in zeolitic imidazolate framework (ZIF) crystals. The molecules are homogeneously distributed within the crystals, and their loadings can be tuned. We show that ZIF-8 crystals loaded with the anticancer drug doxorubicin (DOX) are efficient drug delivery vehicles in cancer therapy using pH-responsive release. Their efficacy on breast cancer cell lines is higher than that of free DOX. Our one-pot process opens new possibilities to construct multifunctional delivery systems for a wide range of applications.

  14. One pot three component reaction for the rapid synthesis of pyrrolo[1,2-a]benzimidazoles.

    PubMed

    Hsu, Wei-Shun; Paike, Vijaykumar; Sun, Chung-Ming

    2013-05-01

    An efficient strategy for the synthesis of pyrrolo[1,2-a]-benzimidazole (PBI) linked to an ionic liquid (ILs) as a soluble support under microwave irradiation was explored. The key intermediate benzimidazoles were synthesized via N-acylation followed by cyclodehydration of IL-supported methyl-3-amino-4-(isobutylamino) benzoate. The synthesis of the IL-bound PBI was performed by one-pot three-component condensation under microwave dielectric heating, which involved a Knoevenagel condensation and a [4+1]-cycloaddition reaction. The reaction was monitored directly by means of (1)H NMR. All final products were obtained in good yield and high purity after precipitation.

  15. Facile one-pot synthesis of porphyrin based porous polymer networks (PPNs) as biomimetic catalysts

    SciTech Connect

    Zou, LF; Feng, DW; Liu, TF; Chen, YP; Fordham, S; Yuan, S; Tian, J; Zhou, HC

    2015-01-01

    Stable porphyrin based porous polymer networks, PPN-23 and PPN-24, have been synthesized through a facile one-pot approach by the aromatic substitution reactions of pyrrole and aldehydes. PPN-24(Fe) shows high catalytic efficiency as a biomimetic catalyst in the oxidation reaction of 2,2'-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid) (ABTS) in the presence of H2O2.

  16. Cell compatible arginine containing cationic polymer: one-pot synthesis and preliminary biological assessment.

    PubMed

    Zavradashvili, Nino; Memanishvili, Tamar; Kupatadze, Nino; Baldi, Lucia; Shen, Xiao; Tugushi, David; Wandrey, Christine; Katsarava, Ramaz

    2014-01-01

    Synthetic cationic polymers are of interest as both nonviral vectors for intracellular gene delivery and antimicrobial agents. For both applications synthetic polymers containing guanidine groups are of special interest since such kind of organic compounds/polymers show a high transfection potential along with antibacterial activity. It is important that the delocalization of the positive charge of the cationic group in guanidine significantly decreases the toxicity compared to the ammonium functionality. One of the most convenient ways for incorporating guanidine groups is the synthesis of polymers composed of the amino acid arginine (Arg) via either application of Arg-based monomers or chemical modification of polymers with derivatives of Arg. It is also important to have biodegradable cationic polymers that will be cleared from the body after their function as transfection or antimicrobial agent is fulfilled. This chapter deals with a two-step/one-pot synthesis of a new biodegradable cationic polymer-poly(ethylene malamide) containing L-arginine methyl ester covalently attached to the macrochains in β-position of the malamide residue via the α-amino group. The goal cationic polymer was synthesized by in situ interaction of arginine methyl ester dihydrochloride with intermediary poly(ethylene epoxy succinimide) formed by polycondensation of di-p-nitrophenyl-trans-epoxy succinate with ethylenediamine. The cell compatibility study with Chinese hamster ovary (CHO) and insect Schneider 2 cells (S2) within the concentration range of 0.02-500 mg/mL revealed that the new polymer is not cytotoxic. It formed nanocomplexes with pDNA (120-180 nm in size) at low polymer/DNA weight ratios (WR = 5-10). A preliminarily transfection efficiency of the Arg-containing new cationic polymer was assessed using CHO, S2, H5, and Sf9 cells.

  17. Titanium-catalyzed multicomponent couplings: efficient one-pot syntheses of nitrogen heterocycles.

    PubMed

    Odom, Aaron L; McDaniel, Tanner J

    2015-11-17

    Nitrogen-based heterocycles are important frameworks for pharmaceuticals, natural products, organic dyes for solar cells, and many other applications. Catalysis for the formation of heterocyclic scaffolds, like many C-C and C-N bond-forming reactions, has focused on the use of rare, late transition metals like palladium and gold. Our group is interested in the use of Earth-abundant catalysts based on titanium to generate heterocycles using multicomponent coupling strategies, often in one-pot reactions. To be of maximal utility, the catalysts need to be easily prepared from inexpensive reagents, and that has been one guiding principle in the research. For this purpose, a series of easily prepared pyrrole-based ligands has been developed. Titanium imido complexes are known to catalyze the hydroamination of alkynes, and this reaction has been used to advantage in the production of α,β-unsaturated imines from 1,3-enynes and pyrroles from 1,4-diynes. Likewise, catalyst design can be used to find complexes applicable to hydrohydrazination, coupling of a hydrazine and alkyne, which is a method for the production of hydrazones. Many of the hydrazones synthesized are converted to indoles through Fischer cyclization by addition of a Lewis acid. However, more complex products are available in a single catalytic cycle through coupling of isonitriles, primary amines, and alkynes to give tautomers of 1,3-diimines, iminoamination (IA). The products of IA are useful intermediates for the one-pot synthesis of pyrazoles, pyrimidines, isoxazoles, quinolines, and 2-amino-3-cyanopyridines. The regioselectivity of the reactions is elucidated in some detail for some of these heterocycles. The 2-amino-3-cyanopyridines are synthesized through isolable intermediates, 1,2-dihydro-2-iminopyridines, which undergo Dimroth rearrangement driven by aromatization of the pyridine ring; the proposed mechanism of the reaction is discussed. The IA-based heterocyclic syntheses can be accomplished

  18. One-Pot Synthesis of Tetraphene and Construction of Expanded Conjugated Aromatics.

    PubMed

    Wang, Jianbo; Yao, Jinzhong; Wang, Hailong; Chen, Hao; Dong, Jingcheng; Zhou, Hongwei

    2016-06-17

    Acene derivatives as a class of polycyclic aromatic hydrocarbons have attracted considerable interest because of their outstanding semiconductor properties. We developed a one-pot synthesis for fully conjugated tetraphene via a sequence of propargyl-allenyl isomerization, phosphine addition, intramolecular Wittig reactions, and Diels-Alder cyclization reactions. The derivative-conjugated aromatic compounds including carbazole or triphenylamine have been constructed via Pd-catalyzed coupling reaction with dibromotetraphene. These compounds show superior photophysical and electrochemical properties, which make them possible candidates for optoelectronic conjugated materials.

  19. A Nitrogen-Assisted One-Pot Heteroaryl Ketone Synthesis from Carboxylic Acids and Heteroaryl Halides.

    PubMed

    Demkiw, Krystyna; Araki, Hirofumi; Elliott, Eric L; Franklin, Christopher L; Fukuzumi, Yoonjoo; Hicks, Frederick; Hosoi, Kazushi; Hukui, Tadashi; Ishimaru, Yoichiro; O'Brien, Erin; Omori, Yoshimasa; Mineno, Masahiro; Mizufune, Hideya; Sawada, Naotaka; Sawai, Yasuhiro; Zhu, Lei

    2016-04-15

    A practical and highly effective one-pot synthesis of versatile heteroaryl ketones directly from carboxylic acids and heteroaryl halides under mild conditions is reported. This method does not require derivatization of carboxylic acids (preparation of acid chlorides, Weinreb amides, etc.) or the use of any additives/catalysts. A wide substrate scope of carboxylic acids with high functional group tolerance has also been demonstrated. The results reveal that the presence of an α-nitrogen on the halide substrate greatly improves the desired ketone formation.

  20. One-pot and two-step synthesis of novel carbonylthioureas and dicarbonyldithioureas derivatives

    NASA Astrophysics Data System (ADS)

    Banaei, Alireza; Shiran, Jafar Abbasi; Saadat, Afshin; Ardabili, Farnaz Fazlalizadeh; McArdle, Patrick

    2015-11-01

    One-pot, two-step synthesis of several 1-cyclopropanecarbonyl-3-(substituted phenyl)-thioureas and 1-(phenylene-1,4-dione)-3,3‧-(substituted phenyl)-dithioureas have been successfully prepared. The structures of the synthesized compounds were confirmed by elemental analysis, FT-IR spectroscopy and NMR. Also the crystal structure one of these compounds was determined by X-ray crystallography. All synthesized compounds were evaluated for antibacterial activity using Salmonella enterica (SE), Micrococcus luteus (ML), Bacillus subtilis (BS) and Pseudomonas aeruginosa (PS).

  1. Facile one-pot synthesis of a polyvinylpyrrolidone-based self-crosslinked fluorescent film.

    PubMed

    Yin, Meizhen; Ye, Yong; Sun, Mengmeng; Kang, Naiwen; Yang, Wantai

    2013-04-12

    A polyvinylpyrrolidone (PVP)-based fluorescent film with stable optical properties is successfully prepared in one pot without any additive. The reaction mechanism of ring-opening and self-crosslinking of linear PVP is proposed and demonstrated. The morphologies and the nanostructures of the fluorescent film as well as the unmodified film are investigated. The dye is incorporated into the film networks via covalent linkages, thus leading to the highly stable optical properties. The facile and effective synthesis approach opens a new way for the design of other multi-functional composite materials based on linear PVP.

  2. The immobilization of 3-(chloropropyl)triethoxysilane onto silica by a simple one-pot synthesis.

    PubMed

    Adam, Farook; Osman, Hasnah; Hello, Kasim Mohammed

    2009-03-01

    Sodium silicate from rice husk ash (RHA) was transformed to functionalized silica with 3-(chloropropyl)triethoxysilane (CPTES) via a simple sol-gel technique in a one-pot synthesis. The (29)Si MAS NMR of the organo-silica complex (RHACCl) showed the presence of T(2), T(3), Q(3) and Q(4) silicon centers. The (13)C MAS NMR showed that RHACCl had three chemical shifts at 10.37, 26.70 and 47.69 ppm consistent with the three carbon atoms of the CPTES moiety. The presence of carbon, silicon and chlorine was determined by a combination of elemental analysis and EDX study.

  3. Gold nanoparticles with cyclic phenylazomethines: one-pot synthesis and metal ion sensing.

    PubMed

    Shomura, Ryo; Chung, Keum Jee; Iwai, Hideo; Higuchi, Masayoshi

    2011-07-01

    New gold nanoparticles covered with cyclic phenylazomethine (CPA) were obtained by a one-pot synthesis. It is confirmed by XPS that imines of CPA in the nanoparticles (Au-CPA) are partially reduced to amines. The amine part of CPA in Au-CPA is attached to the surfaces of gold nanoparticles, and the imine part works as a redox-active site. A glassy carbon electrode modified with Au-CPA was revealed to work as an electrochemical probe for metal ion sensing.

  4. One-Pot, Four-Step Organocatalytic Asymmetric Synthesis of Functionalized Nitrocyclopropanes.

    PubMed

    Zaghi, Anna; Bernardi, Tatiana; Bertolasi, Valerio; Bortolini, Olga; Massi, Alessandro; De Risi, Carmela

    2015-09-18

    The asymmetric synthesis of functionalized nitrocyclopropanes has been achieved by a one-pot, four-step method catalyzed by (S)-diphenylprolinol TMS ether, which joins two sequential domino reactions, namely a domino sulfa-Michael/aldol condensation of α,β-unsaturated aldehydes with 1,4-dithiane-2,5-diol, and a domino Michael/α-alkylation reaction of the derived chiral dihydrothiophenes with bromonitromethane. The title compounds were obtained in 27-45% yields, with high levels of diastereoselectivity (93:7 to 100:0 dr) and generally good enantioselectivities (up to 95:5 er). PMID:26317611

  5. One-pot odourless synthesis of thioesters via in situ generation of thiobenzoic acids using benzoic anhydrides and thiourea

    PubMed Central

    Khalifeh, Reza

    2015-01-01

    Summary An efficient and odourless procedure for a one-pot synthesis of thioesters by the reaction of benzoic anhydrides, thiourea and various organic halides (primary, allylic, and benzylic) or structurally diverse, electron-deficient alkenes (ketones, esters, and nitriles) in the presence of Et3N has been developed. In this method, thiobenzoic acids were in situ generated from the reaction of thiourea with benzoic anhydrides, which were subjected to conjugate addition with electron-deficient alkenes or a nucleophilic displacement reaction with alkyl halides. PMID:26425185

  6. Brönsted Acid-Catalyzed One-Pot Synthesis of Indoles from o-Aminobenzyl Alcohols and Furans

    PubMed Central

    Kuznetsov, Alexey; Makarov, Anton; Rubtsov, Alexandr E.; Butin, Alexander V.; Gevorgyan, Vladimir

    2013-01-01

    Brönsted acid-catalyzed one-pot synthesis of indoles from o-aminobenzyl alcohols and furans has been developed. This method operates via the in situ formation of aminobenzylfuran, followed by its recyclization into the indole core. The method proved to be efficient for substrates possessing different functional groups, including -OMe, -CO2Cy, and -Br. The resulting indoles can easily be transformed into diverse scaffolds, including 2,3- and 1,2-fused indoles, and indole possessing an α,β-unsaturated ketone moiety at the C-2 position. PMID:24255969

  7. One-pot synthesis and antifungal activity against plant pathogens of quinazolinone derivatives containing an amide moiety.

    PubMed

    Zhang, Jin; Liu, Jia; Ma, Yangmin; Ren, Decheng; Cheng, Pei; Zhao, Jiawen; Zhang, Fan; Yao, Yuan

    2016-05-01

    An efficient one-pot, three-component synthesis of quinazolinone derivatives containing 3-acrylamino motif was carried out using CeO2 nanoparticles as catalyst. Thirty-nine synthesized compounds were obtained with satisfied yield and elucidated by spectroscopic analysis. Four phytopathogenic fungi were chosen to test the antifungal activities by minimum inhibitory concentration (MIC) method. Compounds 4ag, 4bb, 4bc showed broad antifungal activities against at least three fungi, and dramatic effects of substituents on the activities were observed. Docking studies were established to explore the potential antifungal mechanism of quinazolinone derivatives as the chitinase inhibitors, and also verified the importance of the amide moiety.

  8. A convenient tandem one-pot synthesis of donor-acceptor-type triphenylene 2,3-dicarboxylic esters from diarylacetylene.

    PubMed

    Feng, Chun; Tian, Xian-Li; Zhou, Jing; Xiang, Shi-Kai; Yu, Wen-Hao; Wang, Bi-Qin; Hu, Ping; Redshaw, Carl; Zhao, Ke-Qing

    2014-09-28

    A tandem one-pot method for the direct synthesis of polysubstituted triphenylene 2,3-dicarboxylic esters with different substitution patterns was developed by enyne metathesis of diarylacetylene, followed by Diels-Alder, aromatization and a cyclization cascade.

  9. Facile One-Pot Synthesis of Tellurium Nanorods as Antioxidant and Anticancer Agents.

    PubMed

    Huang, Wei; Wu, Hualian; Li, Xiaoling; Chen, Tianfeng

    2016-08-19

    Nanorods have been utilized in targeted therapy, controlled release, molecular diagnosis, and molecule imaging owing to their large surface area and optical, magnetic, electronic, and structural properties. However, low stability and complex synthetic methods have substantially limited the application of tellurium nanorods for use as antioxidant and anticancer agents. Herein, a facile one-pot synthesis of functionalized tellurium nanorods (PTNRs) by using a hydrothermal synthetic system with a polysaccharide-protein complex (PTR), which was extracted from Pleurotus tuber-regium, as a capping agent is described. PTNRs remained stable in water and in phosphate-buffered saline and exhibited high hemocompatibility. Interestingly, these nanorods possessed strong antioxidant activity for scavenging 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid radical cation (ABTS(.+) ) and 2,2-diphenyl-1-picrylhydrazylhydrate (DPPH) free radicals and demonstrated novel anticancer activities. However, these nanorods exhibited low cytotoxicity toward normal human cells. In addition, the PTNRs effectively induced a decrease in the mitochondrial membrane potential in a dose-dependent manner, which indicated that mitochondrial dysfunction might play an important role in PTNR-induced apoptosis. Therefore, this study provides a one-pot strategy for the facile synthesis of tellurium nanorods with novel antioxidant and anticancer application potentials. PMID:27325381

  10. Facile One-Pot Synthesis of Tellurium Nanorods as Antioxidant and Anticancer Agents.

    PubMed

    Huang, Wei; Wu, Hualian; Li, Xiaoling; Chen, Tianfeng

    2016-08-19

    Nanorods have been utilized in targeted therapy, controlled release, molecular diagnosis, and molecule imaging owing to their large surface area and optical, magnetic, electronic, and structural properties. However, low stability and complex synthetic methods have substantially limited the application of tellurium nanorods for use as antioxidant and anticancer agents. Herein, a facile one-pot synthesis of functionalized tellurium nanorods (PTNRs) by using a hydrothermal synthetic system with a polysaccharide-protein complex (PTR), which was extracted from Pleurotus tuber-regium, as a capping agent is described. PTNRs remained stable in water and in phosphate-buffered saline and exhibited high hemocompatibility. Interestingly, these nanorods possessed strong antioxidant activity for scavenging 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid radical cation (ABTS(.+) ) and 2,2-diphenyl-1-picrylhydrazylhydrate (DPPH) free radicals and demonstrated novel anticancer activities. However, these nanorods exhibited low cytotoxicity toward normal human cells. In addition, the PTNRs effectively induced a decrease in the mitochondrial membrane potential in a dose-dependent manner, which indicated that mitochondrial dysfunction might play an important role in PTNR-induced apoptosis. Therefore, this study provides a one-pot strategy for the facile synthesis of tellurium nanorods with novel antioxidant and anticancer application potentials.

  11. Synthesis of enantiopure glycidol derivatives via a one-pot two-step enzymatic cascade.

    PubMed

    Liu, Yu-Chang; Liu, Yan; Wu, Zhong-Liu

    2015-02-21

    Styrene monooxygenase (SMO) can catalyze the kinetic resolution of secondary allylic alcohols to provide enantiopure glycidol derivatives. To overcome the low theoretical yield of kinetic resolution, we designed a one-pot two-step enzymatic cascade using prochiral α,β-unsaturated ketones as the substrates. An S-specific ketoreductase ChKRED03 was screened for the efficient bioreduction of the substrates to provide (S)-allylic alcohols, which underwent SMO-catalyzed epoxidation to achieve glycidol derivatives with contiguous stereogenic centers. Excellent enantioselectivity (ee > 99%) and diastereoselectivity (de > 99%) were achieved for the majority of the substrates, and product yields reached up to >99%.

  12. One-pot exfoliation of graphite and synthesis of nanographene/dimesitylporphyrin hybrids.

    PubMed

    Bernal, M Mar; Pérez, Emilio M

    2015-01-01

    A simple one-pot process to exfoliate graphite and synthesize nanographene-dimesitylporphyrin hybrids has been developed. Despite the bulky mesityl groups, which are expected to hinder the efficient π-π stacking between the porphyrin core and graphene, the liquid-phase exfoliation of graphite is significantly favored by the presence of the porphyrins. Metallation of the porphyrin further enhances this effect. The resulting graphene/porphyrin hybrids were characterized by spectroscopy (UV-visible, fluorescence, and Raman) and microscopy (STEM, scanning transmission electron microscopy).

  13. One-Pot Exfoliation of Graphite and Synthesis of Nanographene/Dimesitylporphyrin Hybrids

    PubMed Central

    Bernal, M. Mar; Pérez, Emilio M.

    2015-01-01

    A simple one-pot process to exfoliate graphite and synthesize nanographene-dimesitylporphyrin hybrids has been developed. Despite the bulky mesityl groups, which are expected to hinder the efficient π–π stacking between the porphyrin core and graphene, the liquid-phase exfoliation of graphite is significantly favored by the presence of the porphyrins. Metallation of the porphyrin further enhances this effect. The resulting graphene/porphyrin hybrids were characterized by spectroscopy (UV-visible, fluorescence, and Raman) and microscopy (STEM, scanning transmission electron microscopy). PMID:25984598

  14. One-pot synthesis of CuFeSe{sub 2} cuboid nanoparticles

    SciTech Connect

    Hsu, Yu-Kuei; Lin, Yan-Gu; Chen, Ying-Chu

    2011-11-15

    Graphical abstract: CuFeSe{sub 2} cuboid nanoparticles with a tetragonal phase have been successfully synthesized via chemical route from a nonaqueous solution of octadecylamine solvent and metal chloride of precursor. Highlights: {yields} CuFeSe{sub 2} cuboid nanoparticles were prepared by a cost-effective and simple one-pot chemical route. {yields} Synthesized temperature and octadecylamine solvent play a significant role in the cuboid shape of nanoparticles. {yields} The nanocrystallinity feature and tetragonal phase of the CuFeSe{sub 2} nanoparticles were confirmed by HRTEM. -- Abstract: Ternary semiconducting CuFeSe{sub 2} nanocrystals of a particular shape and size were successfully synthesized using a cost-effective and simple one-pot chemical route. X-ray powder diffraction and field emission scanning electron microscopy results indicated that the as-synthesized CuFeSe{sub 2} comprised cuboid nanoparticles with dimensions of 50-150 nm as well as a tetragonal phase. Elemental analysis yielded an atomic ratio of Cu:Fe:Se of 1:1.06:2.17. The synthesis temperature and the solvent octadecylamine were significant in determining the structural phases and morphologies of the final products. The optimal condition for synthesizing the tetragonal CuFeSe{sub 2} phase with cuboid nanoparticles was a reaction temperature of 200 {sup o}C for 1 h in octadecylamine solvent. A possible mechanism of the formation of ternary CuFeSe{sub 2} nanoparticles with controllable shapes is discussed.

  15. Modular Synthesis of Novel Macrocycles Bearing α,β-Unsaturated Chemotypes through a Series of One-Pot, Sequential Protocols.

    PubMed

    Javed, Salim; Bodugam, Mahipal; Torres, Jessica; Ganguly, Arghya; Hanson, Paul R

    2016-05-10

    A series of one-pot, sequential protocols was developed for the synthesis of novel macrocycles bearing α,β-unsaturated chemotypes. The method highlights a phosphate tether-mediated approach to establish asymmetry, and consecutive one-pot, sequential processes to access the macrocycles with minimal purification procedures. This library amenable strategy provided diverse macrocycles containing α,β-unsaturated carbon-, sulfur-, or phosphorus-based warheads.

  16. A Short, One-Pot Synthesis of Bupropion (Zyban®, Wellbutrin®)

    NASA Astrophysics Data System (ADS)

    Perrine, Daniel M.; Ross, Jason T.; Nervi, Stephen J.; Zimmerman, Richard H.

    2000-11-01

    A one-pot synthesis of (±)-2-(t-butylamino)-3'-chloropropiophenone (bupropion) as its hydrochloride salt (Zyban, Wellbutrin), an important antidepressant drug used in the treatment of nicotine addiction, is described. The procedure, suitable for students in their first year of organic chemistry, can be carried out in less than two hours and provides material of high purity in overall yield of 75-85%. A solution of m-chloropropiophenone in CH2Cl2 is treated with Br2. After removal of the solvent, t-butylamine and N-methylpyrrolidinone are added and the mixture is warmed briefly, quenched with water, and extracted with ether. Concentrated HCl is added to the ether solution to precipitate the product.

  17. One-pot synthesis of PVA-capped silver nanoparticles their characterization and biomedical application

    NASA Astrophysics Data System (ADS)

    Patil, Rupali S.; Kokate, Mangesh R.; Jambhale, Chitra L.; Pawar, Sambhaji M.; Han, Sung H.; Kolekar, Sanjay S.

    2012-03-01

    The rapid one-pot synthesis of silver nanoparticles (SNPs) at room temperature by using hydrazine hydrate as reducing agent and polyvinyl alcohol as stabilizing agent is reported. The SNPs were characterized with UV-visible (UV-Vis) spectroscopy, x-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). The synthesized silver nanoparticle shows surface plasmon resonance at 410 nm. The XRD reveals face-centered cubic (FCC) structure of SNPs. FE-SEM, AFM and TEM show that nanoparticles have spherical morphology with diameters in the range of 10-60 nm. The antimicrobial activity of synthesized hybrid material against strains of four different bacteria (Bacillus cereus, Escherichia coli, Staphylococus aureus, Proteus vulgaris), that are commonly found in hospitals has been studied. The results indicate that such particles have potential applications in biotechnology and biomedical science.

  18. One-pot laser-assisted synthesis of porous carbon with embedded magnetic cobalt nanoparticles

    NASA Astrophysics Data System (ADS)

    Ghimbeu, Camélia Matei; Sopronyi, Mihai; Sima, Felix; Delmotte, Luc; Vaulot, Cyril; Zlotea, Claudia; Paul-Boncour, Valérie; Le Meins, Jean-Marc

    2015-05-01

    A novel one-pot laser-assisted approach is reported herein for the synthesis of ordered carbons with embedded cobalt nanoparticles. The process is based on a UV pulsed laser exposure of an ethanolic solution consisting of green carbon precursors, a structure directing agent and a cobalt salt. Very short irradiation times (5 to 30 min) are only required to polymerize and cross-link carbon precursors (i.e. phloroglucinol and glyoxylic acid) independent of a catalyst presence. The influence of three metallic salts (acetate, nitrate and chloride) on the phenolic resin and carbon characteristics (structure, texture and particle size/distribution) was systematically studied. When exposed to UV laser, the metallic salt exhibited a strong influence on the particle size and distribution in the carbon matrix rather than on the textural carbon properties. Using cobalt acetate, very small (3.5 nm) and uniformly dispersed particles were obtained by this simple, fast and green one-pot synthesis approach. An original combined 13C CP-MAS and DP-DEC solid state NMR spectroscopy analysis allowed to determine the structure of phenolic resins as well as the location of the cobalt salt in the resin. Complementarily, the 1H solid-state and relaxation NMR provided unique insights into the rigidity (cross-linking) of the phenolic resin and dispersion of the cobalt salt. The magnetic properties of cobalt nanoparticles were found to be size-dependent: large Co nanoparticles (~50 nm) behave as bulk Co whereas small Co nanoparticles are superparamagnetic.A novel one-pot laser-assisted approach is reported herein for the synthesis of ordered carbons with embedded cobalt nanoparticles. The process is based on a UV pulsed laser exposure of an ethanolic solution consisting of green carbon precursors, a structure directing agent and a cobalt salt. Very short irradiation times (5 to 30 min) are only required to polymerize and cross-link carbon precursors (i.e. phloroglucinol and glyoxylic acid

  19. Reducing size-dispersion in one-pot aqueous synthesis of maghemite nanoparticles.

    PubMed

    Drummond, A L; Feitoza, N C; Duarte, G C; Sales, M J A; Silva, L P; Chaker, J A; Bakuzis, A F; Sousa, M H

    2012-10-01

    Nanosized maghemite-like particles with reduced size-distribution were obtained using a one-pot synthesis route in aqueous medium. Forced hydrolysis of iron ions in ammoniac solution led to the formation of magnetite nanoparticles that were oxidized to maghemite in a hydrothermal digestion step that reduced the polydispersity of nanograins. The prepared nanoparticles were characterized by chemical analysis, X-ray diffractometry, magnetization, Raman spectroscopy and transmission electron microscopy measurements. Data showed that 14 nm-sized particles with polydispersity of about 0.14 were produced and, differently from other procedures, neither additional steps nor toxic reagents were needed to reduce size-dispersion or to oxidize magnetite to maghemite. These facts per se turn such nanodevice into a good potential choice for biomedical applications.

  20. One-pot microbial synthesis of 2'-deoxyribonucleoside from glucose, acetaldehyde, and a nucleobase.

    PubMed

    Horinouchi, Nobuyuki; Ogawa, Jun; Kawano, Takako; Sakai, Takafumi; Saito, Kyota; Matsumoto, Seiichiro; Sasaki, Mie; Mikami, Yoichi; Shimizu, Sakayu

    2006-06-01

    A one-pot enzymatic synthesis of 2'-deoxyribonucleoside from glucose, acetaldehyde, and a nucleobase was established. Glycolysis by baker's yeast (Saccharomyces cerevisiae) generated ATP which was used to produce D: -glyceraldehyde 3-phosphate production from glucose via fructose 1,6-diphosphate. The D: -glyceraldehyde 3-phosphate produced was transformed to 2'-deoxyribonucleoside via 2-deoxyribose 5-phosphate and then 2-deoxyribose 1-phosphate in the presence of acetaldehyde and a nucleobase by deoxyriboaldolase, phosphopentomutase expressed in Escherichia coli, and a commercial nucleoside phosphorylase. About 33 mM 2'-deoxyinosine was produced from 600 mM glucose, 333 mM acetaldehyde and 100 mM adenine in 24 h. 2'-Deoxyinosine was produced from adenine due to the adenosine deaminase activity of E. coli transformants.

  1. Greener and rapid access to bio-active heterocycles: one-pot solvent-free synthesis of 1,3,4-oxadiazoles and 1,3,4-thiadiazoles

    EPA Science Inventory

    A novel one-pot solvent free synthesis of 1,3,4-oxadiazoles and 1,3,4-thiadiazoles by condensation of acid hydrazide and triethyl orthoalkanates under microwave irradiations is reported. This green protocol was catalyzed efficiently by solid supported Nafion®NR50 and phosphorus p...

  2. One-pot laser-assisted synthesis of porous carbon with embedded magnetic cobalt nanoparticles.

    PubMed

    Ghimbeu, Camélia Matei; Sopronyi, Mihai; Sima, Felix; Delmotte, Luc; Vaulot, Cyril; Zlotea, Claudia; Paul-Boncour, Valérie; Le Meins, Jean-Marc

    2015-06-14

    A novel one-pot laser-assisted approach is reported herein for the synthesis of ordered carbons with embedded cobalt nanoparticles. The process is based on a UV pulsed laser exposure of an ethanolic solution consisting of green carbon precursors, a structure directing agent and a cobalt salt. Very short irradiation times (5 to 30 min) are only required to polymerize and cross-link carbon precursors (i.e. phloroglucinol and glyoxylic acid) independent of a catalyst presence. The influence of three metallic salts (acetate, nitrate and chloride) on the phenolic resin and carbon characteristics (structure, texture and particle size/distribution) was systematically studied. When exposed to UV laser, the metallic salt exhibited a strong influence on the particle size and distribution in the carbon matrix rather than on the textural carbon properties. Using cobalt acetate, very small (3.5 nm) and uniformly dispersed particles were obtained by this simple, fast and green one-pot synthesis approach. An original combined (13)C CP-MAS and DP-DEC solid state NMR spectroscopy analysis allowed to determine the structure of phenolic resins as well as the location of the cobalt salt in the resin. Complementarily, the (1)H solid-state and relaxation NMR provided unique insights into the rigidity (cross-linking) of the phenolic resin and dispersion of the cobalt salt. The magnetic properties of cobalt nanoparticles were found to be size-dependent: large Co nanoparticles (∼50 nm) behave as bulk Co whereas small Co nanoparticles are superparamagnetic. PMID:25981107

  3. One-pot laser-assisted synthesis of porous carbon with embedded magnetic cobalt nanoparticles.

    PubMed

    Ghimbeu, Camélia Matei; Sopronyi, Mihai; Sima, Felix; Delmotte, Luc; Vaulot, Cyril; Zlotea, Claudia; Paul-Boncour, Valérie; Le Meins, Jean-Marc

    2015-06-14

    A novel one-pot laser-assisted approach is reported herein for the synthesis of ordered carbons with embedded cobalt nanoparticles. The process is based on a UV pulsed laser exposure of an ethanolic solution consisting of green carbon precursors, a structure directing agent and a cobalt salt. Very short irradiation times (5 to 30 min) are only required to polymerize and cross-link carbon precursors (i.e. phloroglucinol and glyoxylic acid) independent of a catalyst presence. The influence of three metallic salts (acetate, nitrate and chloride) on the phenolic resin and carbon characteristics (structure, texture and particle size/distribution) was systematically studied. When exposed to UV laser, the metallic salt exhibited a strong influence on the particle size and distribution in the carbon matrix rather than on the textural carbon properties. Using cobalt acetate, very small (3.5 nm) and uniformly dispersed particles were obtained by this simple, fast and green one-pot synthesis approach. An original combined (13)C CP-MAS and DP-DEC solid state NMR spectroscopy analysis allowed to determine the structure of phenolic resins as well as the location of the cobalt salt in the resin. Complementarily, the (1)H solid-state and relaxation NMR provided unique insights into the rigidity (cross-linking) of the phenolic resin and dispersion of the cobalt salt. The magnetic properties of cobalt nanoparticles were found to be size-dependent: large Co nanoparticles (∼50 nm) behave as bulk Co whereas small Co nanoparticles are superparamagnetic.

  4. A concise synthesis of benzimidazoles via the microwave-assisted one-pot batch reaction of amino acids up to a 10-g scale.

    PubMed

    Peng, Pai; Xiong, Jin-Feng; Mo, Guang-Zhen; Zheng, Jia-Li; Chen, Ren-Hong; Chen, Xiao-Yun; Wang, Zhao-Yang

    2014-10-01

    An efficient method for the synthesis of aminomethyl benzimidazoles is developed by using a one-pot batch reaction between amino acids and o-phenylenediamines. This reaction proceeds smoothly in an unmodified household microwave oven, even though scale-up is to 10 g. A desirable method for the quick synthesis of benzimidazoles, which are used as a kind of important intermediates in drug synthesis, is provided by the scale-up utilization of amino acid resource. PMID:25030664

  5. One-pot synthesis of magnetic nanoclusters enabling atherosclerosis-targeted magnetic resonance imaging

    PubMed Central

    Kukreja, Aastha; Lim, Eun-Kyung; Kang, Byunghoon; Choi, Yuna; Lee, Taeksu; Suh, Jin-Suck; Huh, Yong-Min; Haam, Seungjoo

    2014-01-01

    In this study, dextran-encrusted magnetic nanoclusters (DMNCs) were synthesized using a one-pot solution phase method for detection of atherosclerosis by magnetic resonance imaging. Pyrenyl dextran was used as a surfactant because of its electron-stabilizing effect and its amphiphilic nature, rendering the DMNCs stable and water-dispersible. The DMNCs were 65.6±4.3 nm, had a narrow size distribution, and were superparamagnetic with a high magnetization value of 60.1 emu/g. Further, they showed biocompatibility and high cellular uptake efficiency, as indicated by a strong interaction between dextran and macrophages. In vivo magnetic resonance imaging demonstrated the ability of DMNCs to act as an efficient magnetic resonance imaging contrast agent capable of targeted detection of atherosclerosis. In view of these findings, it is concluded that DMNCs can be used as magnetic resonance imaging contrast agents to detect inflammatory disease. PMID:24904209

  6. One-pot synthesis of magnetic nanoclusters enabling atherosclerosis-targeted magnetic resonance imaging.

    PubMed

    Kukreja, Aastha; Lim, Eun-Kyung; Kang, Byunghoon; Choi, Yuna; Lee, Taeksu; Suh, Jin-Suck; Huh, Yong-Min; Haam, Seungjoo

    2014-01-01

    In this study, dextran-encrusted magnetic nanoclusters (DMNCs) were synthesized using a one-pot solution phase method for detection of atherosclerosis by magnetic resonance imaging. Pyrenyl dextran was used as a surfactant because of its electron-stabilizing effect and its amphiphilic nature, rendering the DMNCs stable and water-dispersible. The DMNCs were 65.6±4.3 nm, had a narrow size distribution, and were superparamagnetic with a high magnetization value of 60.1 emu/g. Further, they showed biocompatibility and high cellular uptake efficiency, as indicated by a strong interaction between dextran and macrophages. In vivo magnetic resonance imaging demonstrated the ability of DMNCs to act as an efficient magnetic resonance imaging contrast agent capable of targeted detection of atherosclerosis. In view of these findings, it is concluded that DMNCs can be used as magnetic resonance imaging contrast agents to detect inflammatory disease.

  7. One pot electrochemical synthesis of polymer/CNT/metal nanoparticles for fuel cell applications

    NASA Astrophysics Data System (ADS)

    Ventrapragada, Lakshman; Zhu, Jingyi; Karakaya, Mehmet; Podila, Ramakrishna; Rao, Apparao; Clemson Nanomaterials center Team

    Carbon nanotubes (CNTs) have become a key player in the design of materials for energy applications. They gained their popularity in industrial and scientific research due to their unique properties like excellent conductivity, high surface area, etc. Here we used chemical vapor deposition (CVD) to synthesize two types of CNTs namely, helically coiled CNTs and vertically aligned CNTs. These CNTs were subsequently used to make composites with conducting polymers and metal nanoparticles. One pot electrochemical synthesis was designed to electropolymerize aniline, pyrrole etc. on the surface of the electrode with simultaneous deposition of platinum and gold metal nanoparticles, and CNTs in the polymer matrix. The as synthesized composite materials were characterized with scanning electron microscope for surface morphology and spectroscopic techniques like Raman, UV-Vis for functionality. These were used to study electrocatalytic oxidation of methanol and ethanol for alkaline fuel cell applications. Electrodes fabricated from these composites not only showed good kinetics but also exhibited excellent stability. Uniqueness of this composite lies in its simple two step synthesis and it doesn't involve any surfactants unlike conventional chemical synthesis routes.

  8. Synthesis of l- and d-Ubiquitin by One-Pot Ligation and Metal-Free Desulfurization.

    PubMed

    Huang, Yi-Chao; Chen, Chen-Chen; Gao, Shuai; Wang, Ye-Hai; Xiao, Hua; Wang, Feng; Tian, Chang-Lin; Li, Yi-Ming

    2016-05-23

    Native chemical ligation combined with desulfurization has become a powerful strategy for the chemical synthesis of proteins. Here we describe the use of a new thiol additive, methyl thioglycolate, to accomplish one-pot native chemical ligation and metal-free desulfurization for chemical protein synthesis. This one-pot strategy was used to prepare ubiquitin from two or three peptide segments. Circular dichroism spectroscopy and racemic protein X-ray crystallography confirmed the correct folding of ubiquitin. Our results demonstrate that proteins synthesized chemically by streamlined 9-fluorenylmethoxycarbonyl (Fmoc) solid-phase peptide synthesis coupled with a one-pot ligation-desulfurization strategy can supply useful molecules with sufficient purity for crystallographic studies.

  9. Highly Photoluminescent Molybdenum Oxide Quantum Dots: One-Pot Synthesis and Application in 2,4,6-Trinitrotoluene Determination.

    PubMed

    Xiao, Sai Jin; Zhao, Xiao Jing; Hu, Ping Ping; Chu, Zhao Jun; Huang, Cheng Zhi; Zhang, Li

    2016-03-01

    As a well-studied transition-metal semiconductor material, MoOx has a wider band gap than molybdenum disulfide (MoS2), and its property varies dramatically for the existence of several different allotropes and suboxide phases of molybdenum oxides (MoOx, x < 3). In this manuscript, a one-pot method possessing the advantages of one pot, easily prepared, rapid, and environmentally friendly, has been developed for facile synthesis of highly photoluminescent MoOx quantum dots (MoOx QDs), in which commercial molybdenum disulfide (MoS2) powder and hydrogen peroxide (H2O2) are employed as the precursor and oxidant, respectively. The obtained MoOx QDs can be further utilized as an efficient photoluminescent probe, and a new turn-off sensor is developed for 2,4,6-trinitrotoluene (TNT) determination based on the fact that the photoluminescence of MoOx QDs can be quenched by the Meisenheimer complexes formed in the strong alkali solution through the inner filter effect (IFE). Under the optimal conditions, the decreased photoluminescence of MoOx QDs shows a good linear relationship to the concentration of TNT ranging from 0.5 to 240.0 μM, and the limit of detection was 0.12 μM (3σ/k). With the present turn-off sensor, TNT in river water samples can be rapidly and selectively detected without tedious sample pretreatment processes.

  10. One pot synthesis of Ag nanoparticle modified ZnO microspheres in ethylene glycol medium and their enhanced photocatalytic performance

    SciTech Connect

    Tian Chungui; Li Wei; Pan Kai; Zhang Qi; Tian Guohui; Zhou Wei; Fu Honggang

    2010-11-15

    Ag nanoparticles (NPs) modified ZnO microspheres (Ag/ZnO microspheres) were prepared by a facile one pot strategy in ethylene glycol (EG) medium. The EG played two important roles in the synthesis: it could act as a reaction media for the formation of ZnO and reduce Ag{sup +} to Ag{sup 0}. A series of the characterizations indicated the successful combination of Ag NPs with ZnO microspheres. It was shown that Ag modification could greatly enhance the photocatalytic efficiency of ZnO microspheres by taking the photodegradation of Rhodamine B as a model reaction. With appropriate ratio of Ag and ZnO, Ag/ZnO microspheres showed the better photocatalytic performance than commercial Degussa P-25 TiO{sub 2}. Photoluminescence and surface photovoltage spectra demonstrated that Ag modification could effectively inhibit the recombination of the photoinduced electron and holes of ZnO. This is responsible for the higher photocatalytic activity of Ag/ZnO composites. -- Graphical abstract: A 'one-pot' strategy was developed for preparing the Ag/ZnO microspheres in ethylene glycol. The composites exhibited superior photocatalytic performance for photodegradation of Rhodamine B dye in water. Display Omitted

  11. Symmetry breaking polymerization: one-pot synthesis of plasmonic hybrid Janus nanoparticles.

    PubMed

    Wang, Yanming; Ding, Tao; Baumberg, Jeremy J; Smoukov, Stoyan K

    2015-06-21

    Asymmetric hybrid nanoparticles have many important applications in catalysis, nanomotion, sensing, and diagnosis, however ways to generate the asymmetric hybrid nanoparticles are quite limited and inefficient. Most current methods rely on interfacial adhesion and modification of already formed particles. In this article we report a one-pot, facile and scalable synthesis of anisotropic Au-polymer hybrid nanoparticles via interfacial oxidative dispersion polymerization. The interfacial nucleation and polymerization lead to spontaneous symmetry breaking and formation of the Janus particles. The reaction is initiated by monomer radicals generated by the strong oxidant HAuCl4, which is itself later reduced by the electron-rich monomers to self-nucleate and form Au nanoparticles (NPs). The competition between divinylbenzene adsorption and the PVP capping agent results in effective partial surface wetting, forming asymmetric Au-PDVB hybrid nanoparticles, by confining growth of each material to its own phase. Such spontaneous symmetry breaking, important in morphogenesis, with control over the subsequent growth processes should lead to significant advances in the synthesis of asymmetric nanostructures. PMID:26000977

  12. One-Pot synthesis of phosphorylated mesoporous carbon heterogeneous catalysts with tailored surface acidity

    SciTech Connect

    Fulvio, Pasquale F; Mahurin, Shannon Mark; Mayes, Richard T; Bauer, Christopher; Wang, Xiqing; Veith, Gabriel M; Dai, Sheng

    2012-01-01

    Soft-templated phosphorylated mesoporous carbons with homogeneous distributions of phosphate groups were prepared by a 'one-pot' synthesis method using mixtures of phosphoric acid with hydrochloric, or nitric acids in the presence of Pluronic F127 triblock copolymer. Adjusting the various ratios of phosphoric acid used in these mixtures resulted in carbons with distinct adsorption, structural and surface acidity properties. The pore size distributions (PSDs) from nitrogen adsorption at -196 C showed that mesoporous carbons exhibit specific surface areas as high as 551 m{sup 2}/g and mesopores as large as 13 nm. Both structural ordering of the mesopores and the final phosphate contents were strongly dependent on the ratios of H{sub 3}PO{sub 4} in the synthesis gels, as shown by transmission electron microscopy (TEM), X-ray photoelectron (XPS) and energy dispersive X-ray spectroscopy (EDS). The number of surface acid sites determined from temperature programmed desorption of ammonia (NH{sub 3}-TPD) were in the range of 0.3-1.5 mmol/g while the active surface areas are estimated to comprise 5-54% of the total surface areas. Finally, the conversion temperatures for the isopropanol dehydration were lowered by as much as 100 C by transitioning from the least acidic to the most acidic catalysts surface.

  13. Symmetry breaking polymerization: one-pot synthesis of plasmonic hybrid Janus nanoparticles.

    PubMed

    Wang, Yanming; Ding, Tao; Baumberg, Jeremy J; Smoukov, Stoyan K

    2015-06-21

    Asymmetric hybrid nanoparticles have many important applications in catalysis, nanomotion, sensing, and diagnosis, however ways to generate the asymmetric hybrid nanoparticles are quite limited and inefficient. Most current methods rely on interfacial adhesion and modification of already formed particles. In this article we report a one-pot, facile and scalable synthesis of anisotropic Au-polymer hybrid nanoparticles via interfacial oxidative dispersion polymerization. The interfacial nucleation and polymerization lead to spontaneous symmetry breaking and formation of the Janus particles. The reaction is initiated by monomer radicals generated by the strong oxidant HAuCl4, which is itself later reduced by the electron-rich monomers to self-nucleate and form Au nanoparticles (NPs). The competition between divinylbenzene adsorption and the PVP capping agent results in effective partial surface wetting, forming asymmetric Au-PDVB hybrid nanoparticles, by confining growth of each material to its own phase. Such spontaneous symmetry breaking, important in morphogenesis, with control over the subsequent growth processes should lead to significant advances in the synthesis of asymmetric nanostructures.

  14. Bifunctional Mesoporous Carbon Nitride: Highly Efficient Enzyme-like Catalyst for One-pot Deacetalization-Knoevenagel Reaction

    PubMed Central

    Zhong, Lin; Anand, Chokkalingam; Lakhi, Kripal Singh; Lawrence, Geoffrey; Vinu, Ajayan

    2015-01-01

    Recently, mesoporous carbon nitride (MCN) has aroused extensive interest for its potential applications in organocatalysis, photo- and electrochemistry and CO2 capture. However, further surface functionalization of MCN for advanced nanomaterials and catalysis still remains very challenging. Here we show that acidic carboxyl groups can be smoothly introduced onto the surface of well-ordered MCN without annihilation between the introduced acid groups and MCN’s inherent basic groups through a facile UV light oxidation method. The functionalization generates a novel bifunctional nanocatalyst which offers an enzyme-like catalytic performance in the one-pot deacetalization-Knoevenagel reaction of benzaldehyde dimethylacetal and malononitrile with 100% conversion and more than 99% selectivity due to the cooperative catalysis between the acid and base groups separated on the surface of the catalyst. The results provide a general method to create multifunctional nanomaterials and open new opportunities for the development of high efficient catalyst for green organic synthesis. PMID:26243180

  15. Bifunctional Mesoporous Carbon Nitride: Highly Efficient Enzyme-like Catalyst for One-pot Deacetalization-Knoevenagel Reaction

    NASA Astrophysics Data System (ADS)

    Zhong, Lin; Anand, Chokkalingam; Lakhi, Kripal Singh; Lawrence, Geoffrey; Vinu, Ajayan

    2015-08-01

    Recently, mesoporous carbon nitride (MCN) has aroused extensive interest for its potential applications in organocatalysis, photo- and electrochemistry and CO2 capture. However, further surface functionalization of MCN for advanced nanomaterials and catalysis still remains very challenging. Here we show that acidic carboxyl groups can be smoothly introduced onto the surface of well-ordered MCN without annihilation between the introduced acid groups and MCN’s inherent basic groups through a facile UV light oxidation method. The functionalization generates a novel bifunctional nanocatalyst which offers an enzyme-like catalytic performance in the one-pot deacetalization-Knoevenagel reaction of benzaldehyde dimethylacetal and malononitrile with 100% conversion and more than 99% selectivity due to the cooperative catalysis between the acid and base groups separated on the surface of the catalyst. The results provide a general method to create multifunctional nanomaterials and open new opportunities for the development of high efficient catalyst for green organic synthesis.

  16. Bifunctional Mesoporous Carbon Nitride: Highly Efficient Enzyme-like Catalyst for One-pot Deacetalization-Knoevenagel Reaction.

    PubMed

    Zhong, Lin; Anand, Chokkalingam; Lakhi, Kripal Singh; Lawrence, Geoffrey; Vinu, Ajayan

    2015-08-05

    Recently, mesoporous carbon nitride (MCN) has aroused extensive interest for its potential applications in organocatalysis, photo- and electrochemistry and CO2 capture. However, further surface functionalization of MCN for advanced nanomaterials and catalysis still remains very challenging. Here we show that acidic carboxyl groups can be smoothly introduced onto the surface of well-ordered MCN without annihilation between the introduced acid groups and MCN's inherent basic groups through a facile UV light oxidation method. The functionalization generates a novel bifunctional nanocatalyst which offers an enzyme-like catalytic performance in the one-pot deacetalization-Knoevenagel reaction of benzaldehyde dimethylacetal and malononitrile with 100% conversion and more than 99% selectivity due to the cooperative catalysis between the acid and base groups separated on the surface of the catalyst. The results provide a general method to create multifunctional nanomaterials and open new opportunities for the development of high efficient catalyst for green organic synthesis.

  17. Nano-ZnO catalyzed multicomponent one-pot synthesis of novel spiro(indoline-pyranodioxine) derivatives.

    PubMed

    Sachdeva, Harshita; Saroj, Rekha; Dwivedi, Diksha

    2014-01-01

    A simple catalytic protocol for the synthesis of novel spiro[indoline-pyranodioxine] derivatives has been developed using ZnO nanoparticle as an efficient, green, and reusable catalyst. The derivatives are obtained in moderate to excellent yield by one-pot three-component reaction of an isatin, malononitrile/ethylcyanoacetate, and 2,2-dimethyl-1,3-dioxane-4,6-dione in absolute ethanol under conventional heating and microwave irradiation. The catalyst was recovered by filtration from the reaction mixture and reused during five consecutive runs without any apparent loss of activity for the same reaction. The mild reaction conditions and recyclability of the catalyst make it environmentally benign synthetic procedure. PMID:24683341

  18. Nano-ZnO Catalyzed Multicomponent One-Pot Synthesis of Novel Spiro(indoline-pyranodioxine) Derivatives

    PubMed Central

    Sachdeva, Harshita; Saroj, Rekha; Dwivedi, Diksha

    2014-01-01

    A simple catalytic protocol for the synthesis of novel spiro[indoline-pyranodioxine] derivatives has been developed using ZnO nanoparticle as an efficient, green, and reusable catalyst. The derivatives are obtained in moderate to excellent yield by one-pot three-component reaction of an isatin, malononitrile/ethylcyanoacetate, and 2,2-dimethyl-1,3-dioxane-4,6-dione in absolute ethanol under conventional heating and microwave irradiation. The catalyst was recovered by filtration from the reaction mixture and reused during five consecutive runs without any apparent loss of activity for the same reaction. The mild reaction conditions and recyclability of the catalyst make it environmentally benign synthetic procedure. PMID:24683341

  19. One-pot synthesis of fluorescent oligonucleotide Ag nanoclusters for specific and sensitive detection of DNA.

    PubMed

    Lan, Guo-Yu; Chen, Wei-Yu; Chang, Huan-Tsung

    2011-01-15

    In this study, we prepared fluorescent, functional oligonucleotide-stabilized silver nanoclusters (FFDNA-Ag NCs) through one-pot synthesis and then employed them as probes for single nucleotide polymorphisms (SNPs). The FFDNA-Ag NCs were obtained through the NaBH(4)-mediated reduction of AgNO(3) in the presence of a DNA strand having the sequence 5'-C(12)-CCAGATACTCACCGG-3'. The specific DNA scaffold combines a fluorescent base motif (C(12)) and a specific sequence (CCAGATACTCACCGG) that recognizes a gene for fumarylacetoacetate hydrolase (FAH). The sensing mechanism of our new probe is based on the FFDNA-Ag NCs having different stabilities (fluorescence intensities) in solutions containing 150 mM NaCl in the absence and presence of perfect match DNA (DNA(pmt)). Under the optimal conditions (150 mM NaCl, 20 mM phosphate solution, pH 7.0), the fluorescence ratios of the FFDNA-Ag NC probes in the presence and absence of DNA(pmt), plotted against the concentration of DNA(pmt), was linear over the range 25-1000 nM (R(2)=0.98), with a limit of detection (S/N=3) of 14 nM. This cost-effective and simple FFDNA-Ag NC probe is sensitive and selective for SNPs of a gene for FAH.

  20. Photothermal cancer therapy using graphitic carbon–coated magnetic particles prepared by one-pot synthesis

    PubMed Central

    Lee, Hyo-Jeong; Sanetuntikul, Jakkid; Choi, Eun-Sook; Lee, Bo Ram; Kim, Jung-Hee; Kim, Eunjoo; Shanmugam, Sangaraju

    2015-01-01

    We describe here a simple synthetic strategy for the fabrication of carbon-coated Fe3O4 (Fe3O4@C) particles using a single-component precursor, iron (III) diethylenetriaminepentaacetic acid complex. Physicochemical analyses revealed that the core of the synthesized particles consists of ferromagnetic Fe3O4 material ranging several hundred nanometers, embedded in nitrogen-doped graphitic carbon with a thickness of ~120 nm. Because of their photothermal activity (absorption of near-infrared [NIR] light), the Fe3O4@C particles have been investigated for photothermal therapeutic applications. An example of one such application would be the use of Fe3O4@C particles in human adenocarcinoma A549 cells by means of NIR-triggered cell death. In this system, the Fe3O4@C can rapidly generate heat, causing >98% cell death within 10 minutes under 808 nm NIR laser irradiation (2.3 W cm−2). These Fe3O4@C particles provided a superior photothermal therapeutic effect by intratumoral delivery and NIR irradiation of tumor xenografts. These results demonstrate that one-pot synthesis of carbon-coated magnetic particles could provide promising materials for future clinical applications and encourage further investigation of this simple method. PMID:25565819

  1. Photothermal cancer therapy using graphitic carbon-coated magnetic particles prepared by one-pot synthesis.

    PubMed

    Lee, Hyo-Jeong; Sanetuntikul, Jakkid; Choi, Eun-Sook; Lee, Bo Ram; Kim, Jung-Hee; Kim, Eunjoo; Shanmugam, Sangaraju

    2015-01-01

    We describe here a simple synthetic strategy for the fabrication of carbon-coated Fe3O4 (Fe3O4@C) particles using a single-component precursor, iron (III) diethylenetriaminepentaacetic acid complex. Physicochemical analyses revealed that the core of the synthesized particles consists of ferromagnetic Fe3O4 material ranging several hundred nanometers, embedded in nitrogen-doped graphitic carbon with a thickness of ~120 nm. Because of their photothermal activity (absorption of near-infrared [NIR] light), the Fe3O4@C particles have been investigated for photothermal therapeutic applications. An example of one such application would be the use of Fe3O4@C particles in human adenocarcinoma A549 cells by means of NIR-triggered cell death. In this system, the Fe3O4@C can rapidly generate heat, causing >98% cell death within 10 minutes under 808 nm NIR laser irradiation (2.3 W cm(-2)). These Fe3O4@C particles provided a superior photothermal therapeutic effect by intratumoral delivery and NIR irradiation of tumor xenografts. These results demonstrate that one-pot synthesis of carbon-coated magnetic particles could provide promising materials for future clinical applications and encourage further investigation of this simple method.

  2. Formation mechanism and size control in one-pot synthesis of mercapto-silica colloidal spheres.

    PubMed

    Lu, Zhenda; Sun, Lei; Nguyen, Kevin; Gao, Chuanbo; Yin, Yadong

    2011-04-01

    Mercapto-silica spheres with controllable size from ∼150 nm to ∼3.5 μm and narrow size distribution have been prepared in water using a one-pot synthesis, in which 3-mercaptopropyltrimethoxysilane (MPS) was used as the sole silica source and ammonia as the base catalyst. The hydrolysis of MPS at the early stage of the reaction produces amphiphilic silicate species which initiate the self-emulsification of the system and lead to the formation of oil-in-water emulsion droplets. Further hydrolysis and condensation promote the nucleation and growth of the mercapto-silica spheres inside the emulsion droplets. These mercapto-silica spheres are both structurally and functionally different from typical silica particles prepared from silicon alkoxides. Understanding the formation mechanism allows systematic tuning of the size of mercapto-silica spheres in a wide range by changing the amount of precursor, the concentration of ammonia, the amount of additional surfactants, and the reaction time. We find that Ostwald ripening may occur quickly if the spheres are kept in the reaction solution, resulting in significant broadening of the particle size distribution. In order to obtain uniform and stable samples, it is important to quench the growth of the mercapto-silica spheres by separating them from the original reaction mixture and then storing them in solvents that can prevent further ripening.

  3. One-pot synthesis and transfer of PMMA/Ag photonic nanocomposites by pulsed laser deposition

    NASA Astrophysics Data System (ADS)

    Karoutsos, V.; Koutselas, I.; Orfanou, P.; Mpatzaka, Th.; Vasileiadis, M.; Vassilakopoulou, A.; Vainos, N. A.; Perrone, A.

    2015-08-01

    Nanocomposite films comprising metallic nanoparticles in polymer matrices find increasing use in emerging photonic, electronic and microsystem applications owing to their tailored advanced functionalities. The versatile development of such films based on poly-methyl-methacrylate (PMMA) matrix having embedded Ag nanoparticles is addressed here. Two low-cost one-pot chemical methods for the synthesis of bulk target nanocomposite materials are demonstrated. These nanocomposites are subsequently transferred via pulsed laser deposition using 193 nm ArF excimer laser radiation, producing films maintaining the structural and functional properties. Both target- and laser-deposited materials have been thoroughly characterized using microscopic, spectroscopic and thermal analysis methods. Infrared spectra demonstrated the close molecular PMMA chain similarity for both target and film materials, though structural alterations identified by thermal analysis proved the enhanced characteristics of films grown. High-resolution electron microscopy proved the transfer of Ag nanoparticles sized 10-50 nm. Visible absorption peaked in the spectral range of 430-440 nm and attributed to the Ag nanocomposite plasmonic response verifying the transfer of the functional performance from target to film.

  4. Four coordination polymers derived from a one-pot reaction and their controlled synthesis.

    PubMed

    Yan, Wei; Hao, Han; Zheng, Hegen

    2016-04-21

    Four different Co(ii) coordination polymers have been built by two flexible ligands 4,4'-dicarboxydiphenyl sulfone (4,4'-sdb) and 1,4-bis((1H-imidazol-1-yl)methyl) benzene (BMB) in a one-pot solvothermal reaction. The structures of and are new, and and have been reported. The crystal structures of were obtained, namely [Co(4,4'-sdb)(BMB)]n (), {[Co2(4,4'-sdb)2(BMB)]·2H2O}n (), and [Co3(4,4'-sdb)2(DMF)(H2O)3]n (), but was confirmed by PXRD. Both and are 2D layered structures with sql topology and their point symbol is {4(4)·6(2)}. These complexes have been characterized by single crystal X-ray diffraction, infrared spectroscopy, thermogravimetry, elemental analysis, and powder X-ray diffraction measurements. By changing the synthesis conditions, four different Co(ii) coordination polymers can be obtained respectively. PMID:26948000

  5. One-pot hydrothermal synthesis of orange fluorescent silver nanoclusters as a general probe for sulfides.

    PubMed

    Lan, Jing; Zhang, Pu; Wang, Ting Ting; Chang, Yong; Lie, Shao Qing; Wu, Zhu Lian; Liu, Zhong De; Li, Yuan Fang; Huang, Cheng Zhi

    2014-07-01

    Water-soluble fluorescent silver nanoclusters (AgNCs) with almost seven and nine silver atoms and a quantum yield (QY) of 5.38 ± 0.25% were successfully prepared via one-pot hydrothermal synthesis using polymethacrylic acid sodium salt (PMAA-Na) as a template. The as-prepared PMAA-AgNCs displayed a mono-distribution, they were uniform in size and the color of the fluorescence, emitting at 579 nm, was orange when excited at 502 nm. What is more, we found that the as-prepared PMAA-AgNCs could be quenched by sulfides based on the formation of a metal-ligand bond Ag-S, and thus sulfides could be sensitively detected by spectrofluorometry. As proof of concept, thiourea (TU) and other sulfides including cysteine (Cys), glutathione (GSH) and dl-methionine could be detected. For example, the color of the orange fluorescent AgNCs solutions darkened upon the addition of TU and the fluorescence of PMAA-AgNCs was quenched. The detection limit for TU was 6.10 μM in the linear range from 8.57 μM to 2.29 mM. PMID:24834451

  6. One-pot synthesis of (-)-oseltamivir and mechanistic insights into the organocatalyzed Michael reaction.

    PubMed

    Mukaiyama, Takasuke; Ishikawa, Hayato; Koshino, Hiroyuki; Hayashi, Yujiro

    2013-12-23

    The one-pot sequential synthesis of (-)-oseltamivir has been achieved without evaporation or solvent exchange in 36% yield over seven reactions. The key step was the asymmetric Michael reaction of pentan-3-yloxyacetaldehyde with (Z)-N-2-nitroethenylacetamide, catalyzed by a diphenylprolinol silyl ether. The use of a bulky O-silyl-substituted diphenylprolinol catalyst, chlorobenzene as a solvent, and HCO2 H as an acid additive, were key to produce the first Michael adduct in both excellent yield and excellent diastereo- and enantioselectivity. Investigation into the effect of acid demonstrated that an acid additive accelerates not only the E-Z isomerization of the enamines derived from pentan-3-yloxyacetaldehyde with diphenylprolinol silyl ether, but also ring opening of the cyclobutane intermediate and the addition reaction of the enamine to (Z)-N-2-nitroethenylacetamide. The transition-state model for the Michael reaction of pentan-3-yloxyacetaldehyde with (Z)-N-2-nitroethenylacetamide was proposed by consideration of the absolute configuration of the major and minor isomers of the Michael product with the results of the Michael reaction of pentan-3-yloxyacetaldehyde with phenylmaleimide and naphthoquinone.

  7. Efficient production of biodiesel from waste grease: one-pot esterification and transesterification with tandem lipases.

    PubMed

    Yan, Jinyong; Li, Aitao; Xu, Yi; Ngo, Thao P N; Phua, Szechao; Li, Zhi

    2012-11-01

    A novel concept and efficient method for producing biodiesel (FAME) from grease (15-40wt% free fatty acid, FFA) were developed by using tandem lipases for one-pot esterification of FFA and transesterification of triglyceride with methanol in a solvent-free system. Combining immobilized Candida antarctica lipase B (CALB) (Novozyme 435) favoring the esterification and immobilized Thermomyces lanuginosus lipase (TLL) (Lipozyme TLIM) preferring the transesterification at 2:8 (wt/wt) gave FAME in 80% yield, being better than that with Novozyme 435 or Lipozyme TLIM. Recombinant Escherichia coli (Calb/Tll) co-expressing CALB and TLL was engineered as a more efficient tandem-lipases system. Using wet or dry cells (4wt%) gave FAME in 87% or 95% yield, which is much better than that with E. coli cells expressing either CALB or TLL alone. Cells of E. coli (Calb/Tll) were recycled for five times and retained 75% productivity, thus being practical for producing biodiesel from grease.

  8. Efficient production of biodiesel from waste grease: one-pot esterification and transesterification with tandem lipases.

    PubMed

    Yan, Jinyong; Li, Aitao; Xu, Yi; Ngo, Thao P N; Phua, Szechao; Li, Zhi

    2012-11-01

    A novel concept and efficient method for producing biodiesel (FAME) from grease (15-40wt% free fatty acid, FFA) were developed by using tandem lipases for one-pot esterification of FFA and transesterification of triglyceride with methanol in a solvent-free system. Combining immobilized Candida antarctica lipase B (CALB) (Novozyme 435) favoring the esterification and immobilized Thermomyces lanuginosus lipase (TLL) (Lipozyme TLIM) preferring the transesterification at 2:8 (wt/wt) gave FAME in 80% yield, being better than that with Novozyme 435 or Lipozyme TLIM. Recombinant Escherichia coli (Calb/Tll) co-expressing CALB and TLL was engineered as a more efficient tandem-lipases system. Using wet or dry cells (4wt%) gave FAME in 87% or 95% yield, which is much better than that with E. coli cells expressing either CALB or TLL alone. Cells of E. coli (Calb/Tll) were recycled for five times and retained 75% productivity, thus being practical for producing biodiesel from grease. PMID:22940338

  9. One-pot, sequential four-component synthesis of benzo[c]pyrano[3,2-a]phenazine, bis-benzo[c]pyrano[3,2-a]phenazine and oxospiro benzo[c]pyrano[3,2-a]phenazine derivatives using 1,4-diazabicyclo[2.2.2]octane (DABCO) as an efficient and reusable solid base catalyst.

    PubMed

    Hasaninejad, Alireza; Firoozi, Somayeh

    2013-08-01

    1,4-Diazabicyclo[2.2.2]octane (DABCO) has been used as an efficient and reusable solid base catalyst for the one-pot, two-step, four-component synthesis of pyrano[3,2-a]phenazine derivatives by the condensation reaction of 2-hydroxy-1,4-naphthoquinone, 1,2-diamines, carbonyl compounds and alkylmalonates under conventional heating as well as microwave irradiation. This procedure has also been applied successfully for the synthesis of novel bis- benzo[c]pyrano[3,2-a]phenazine and oxospiro benzo[c]pyrano[3,2-a]phenazine derivatives. Using this procedure, all the products were obtained in good to excellent yields. The catalyst has been recovered and reused several times without any loss of reactivity.

  10. Brønsted Acid-Promoted One-Pot Synthesis of Chrysene Derivatives via Isochromenylium Intermediate Formed in Situ.

    PubMed

    Guo, Biao; Zhou, Yiming; Zhang, Lei; Hua, Ruimao

    2015-08-01

    Trifluoromethanesulfonic acid (HOTf) promoted cross-coupling of ortho-[2-(4-methoxylphenyl)-alkynyl]acetophenones with ortho-alkynylbenzaldehydes affording chrysene derivatives has been developed. The present cascade reaction provides a facile one-pot synthesis of multisubstituted chrysenes as well as naked chrysene under mild conditions. The mechanism experimental results demonstrate isochromenylium is a key intermediate for this transformation.

  11. Stereo- and regio-selective one-pot synthesis of triazole-based unnatural amino acids and β- amino triazoles

    EPA Science Inventory

    Synthesis of triazole based unnatural amino acids and β-amino triazole has been described via stereo and regioselective one-pot multi-component reaction of sulfamidates, sodium azide, and alkynes under MW conditions. The developed method is applicable to a broad substrate scope a...

  12. A facile one-pot synthesis of ruthenium hydroxide nanoparticles on magnetic silica: Aqueous hydration of nitriles to amides

    EPA Science Inventory

    One-pot synthesis of ruthenium hydroxide nanoparticles on magnetic silica is described which involve the in situ generation of magnetic silica (Fe3O4@ SiO2) and ruthenium hydroxide immobilization; the hydration of nitriles occurs in high yield and excellent selectivity using this...

  13. A one-pot synthesis of polysulfane-bearing block copolymer nanoparticles with tunable size and refractive index.

    PubMed

    Lim, Jeewoo; Cho, Yunshik; Kang, Eun-Hye; Yang, Sanghee; Pyun, Jeffrey; Choi, Tae-Lim; Char, Kookheon

    2016-02-11

    A one-pot synthesis of sulfur-rich polymer nanoparticles through a ring-opening metathesis polymerization is reported. The nanoparticles are formed in situ from diblock copolymers containing a polynorbornene derivative bearing cyclic polysulfanes. The refractive indices of the resulting nanoparticles are readily controlled in the range from 1.54 to nearly 1.65.

  14. Metal-free one-pot synthesis of 2-substituted and 2,3-disubstituted morpholines from aziridines.

    PubMed

    Sun, Hongnan; Huang, Binbin; Lin, Run; Yang, Chao; Xia, Wujiong

    2015-01-01

    The metal-free synthesis of 2-substituted and 2,3-disubstituted morpholines through a one-pot strategy is described. A simple and inexpensive ammonium persulfate salt enables the reaction of aziridines with halogenated alcohols to proceed via an SN2-type ring opening followed by cyclization of the resulting haloalkoxy amine. PMID:25977727

  15. One-pot synthesis of magnetically recyclable mesoporous silica supported acid-base catalysts for tandem reactions.

    PubMed

    Jun, Samuel Woojoo; Shokouhimehr, Mohammadreza; Lee, Dong Jun; Jang, Youngjin; Park, Jinkyung; Hyeon, Taeghwan

    2013-09-14

    We report one-pot synthesis of magnetically recyclable mesoporous silica catalysts for tandem acid-base reactions. The catalysts could be easily recovered from the reaction mixture using a magnet, and the pore size of the catalysts could be controlled by introducing a swelling agent, resulting in the significant enhancement of the reaction rate.

  16. An Efficient One-Pot Green Protocol for the Synthesis of 5-Unsubstituted 3,4-Dihydropyrimidin-2(1H)-Ones Using Recyclable Amberlyst 15 DRY as a Heterogeneous Catalyst via Three-Component Biginelli-Like Reaction

    PubMed Central

    Jetti, Srinivasa Rao; Verma, Divya; Jain, Shubha

    2012-01-01

    An environmentally benign green protocol for the synthesis of 5-unsubstituted 3,4-dihydropyrimidin-2(1H)-ones using Amberlyst 15 DRY as a recyclable catalyst has been developed. The use of resinous, nontoxic, thermally stable, and inexpensive Amberlyst 15 DRY, as a recyclable heterogeneous catalyst, makes the process simple with negligible chemical waste. Among the various solid acid catalysts Amberlyst 15 DRY was found to be the most efficient catalyst with regard to reaction time, yield, and ease of work-up procedure. PMID:24052845

  17. One-pot reverse microemulsion synthesis of core-shell structured YVO4:Eu3+@SiO2 nanocomposites

    NASA Astrophysics Data System (ADS)

    Liu, Lina; Yue, Surong; Zhang, Yongsheng; Qin, Ruifei; Liu, Lishuang; Zhang, Dongmei; Sun, Ruirui; Chen, Linfeng

    2015-01-01

    Core-shell structured YVO4:Eu3+@SiO2 nanocomposite particles were synthesized using a one-pot reverse microemulsion method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), UV absorption spectra, and photoluminescent spectra. The nanocomposite particles are well-dispersed and about 20 nm in average size. The synthesis method is of one-pot, simplifying the preparation of this kind of core-shell structured nanocomposites. The formation process of these nanocomposite particles is suggested and the photoluminescence properties of them are studied and compared with those of uncoated YVO4:Eu3+ sample.

  18. TiO2 Hollow Spheres: One-Pot Synthesis and Enhanced Photocatalysis

    NASA Astrophysics Data System (ADS)

    Jia, Changchao; Cao, Yongqiang; Yang, Ping

    2013-06-01

    Hollow TiO2 microspheres were successfully fabricated by metal salts with low solubility in ethanol acting as intelligent templates using a simple one-pot solvothermal method. Hollow spheres with large diameter were obtained using CuSO4ṡ5H2O as templates while small ones were obtained using Sr(NO3)2 as templates. It is found that titanium precursor plays an important role for the morphology of samples. Solid TiO2 microspheres were prepared by using titanium tetrabutoxide (TBT). In contrast, bowl-like hollow microspheres were obtained by using titanium tetrachloride (TiCl4). Furthermore, the amount of H2O can stimulate the hydrolysis rate of TiCl4 to form solid spheres. Compared with solid microspheres, hollow TiO2 microspheres depending on their interior cavity structure exhibited enhanced photocatalysis efficiency for the UV-light photodegradation of methyl orange. Quantificationally, the apparent photocatalytic degradation pseudo-first-rate constant of the hollow microspheres is 1.25 times of that of the solid ones.

  19. Synthesis of 5-Amino-2,5-dihydro-1H-benzo[b]azepines Using a One-Pot Multibond Forming Process.

    PubMed

    Sharif, Salaheddin A I; Calder, Ewen D D; Delolo, Fábio G; Sutherland, Andrew

    2016-08-01

    Rapid access to allylic trichloroacetimidates bearing a 2-allylaminoaryl group from readily available 2-iodoanilines combined with a one-pot multibond forming process has allowed the efficient synthesis of a series of 5-amino-2,5-dihydro-1H-benzo[b]azepines. The potential of these compounds as synthetic building blocks was demonstrated by the preparation of a late-stage intermediate of the hyponatremia agent, mozavaptan. PMID:27414232

  20. One-pot approach for synthesis of N-doped TiO2/ZnFe2O4 hybrid as an efficient photocatalyst for degradation of aqueous organic pollutants.

    PubMed

    Yao, Yunjin; Qin, Jiacheng; Chen, Hao; Wei, Fengyu; Liu, Xueting; Wang, Jianlong; Wang, Shaobin

    2015-06-30

    N-doped TiO2/ZnFe2O4 catalysts were successfully prepared by coupling nitrogen modified TiO2 with ZnFe2O4 via a one-pot vapor-thermal method. The physicochemical properties of the as-prepared catalysts have been characterized using various spectroscopic and microscopic techniques. The UV-vis-light-driven photocatalytic activities of the hybrids were evaluated and the effects of the amount of photocatalyst, different types of dyes, catalyst stability on photodegradation of organic dyes were investigated. Moreover, degradation kinetics and mechanism as well as the roles of N doping, ZnFe2O4 and TiO2 have been analyzed. It was revealed that N-doped TiO2/ZnFe2O4 exhibited an improved performance compared with TiO2/ZnFe2O4 or ZnFe2O4 because of the formation of a heterostructure at the interface as well as the introduction of N species. Active species such as holes, electrons, hydroxyl radicals, and superoxide radicals involved in the photodegradation process were detected by using different types of scavengers. Because of ZnFe2O4 in the hybrid, the catalyst shows ferromagnetism, and thus, the hybrid catalyst is easily isolated from the reaction mixture after the photocatalytic experiments. This work not only offers a simple method for the fabrication of N doped TiO2/ZnFe2O4 hybrids, but also provides an effective and conveniently recyclable photocatalyst for the purification of water.

  1. One pot synthesis of cyclohexanone oxime from nitrobenzene using a bifunctional catalyst.

    PubMed

    Rubio-Marqués, Paula; Hernández-Garrido, Juan Carlos; Leyva-Pérez, Antonio; Corma, Avelino

    2014-02-18

    Cyclohexanone oxime is formed from nitrobenzene with 97% yield in a one-pot reaction catalysed by palladium and gold nanoparticles on carbon. The reaction is carried out under hydrogen at 60 °C and the overall transformation involves a multi-step catalysed mechanism from which intermediates and catalytically active species have been identified.

  2. A facile one-pot synthesis of deep blue luminescent lead bromide perovskite microdisks.

    PubMed

    Yuan, Zhao; Shu, Yu; Tian, Yu; Xin, Yan; Ma, Biwu

    2015-11-25

    We report a facile one-pot synthetic method to prepare highly luminescent layered lead(II) bromide perovskite microdisks with the lateral size of a few micrometers and thickness of 100-150 nm, featuring narrow deep blue emissions with quantum yields of up to 53% in toluene solutions and thin films at room temperature.

  3. A rare γ-pyranopyrazole skeleton: design, one-pot synthesis and computational study.

    PubMed

    Üçüncü, Muhammed; Cantürk, Ceren; Karakuş, Erman; Zeybek, Hüseyin; Bozkaya, Uğur; Soydaş, Emine; Şahin, Ertan; Emrullahoğlu, Mustafa

    2016-08-21

    Drawing upon a consecutive amide coupling and intramolecular cyclisation pathway, a one-pot, straightforward synthetic route has been developed for a range of pyrazole fused γ-pyrone derivatives. The reaction mechanism proposed for the chemoselective formation of γ-pyranopyrazole is furthermore fully supported by experimental and computational studies. PMID:27405663

  4. One-pot synthesis of polyunsaturated fatty acid amides with anti-proliferative properties.

    PubMed

    Tremblay, Hugo; St-Georges, Catherine; Legault, Marc-André; Morin, Caroline; Fortin, Samuel; Marsault, Eric

    2014-12-15

    A one-pot environmentally friendly transamidation of ω-3 fatty acid ethyl esters to amides and mono- or diacylglycerols was investigated via the use of a polymer-supported lipase. The method was used to synthesize a library of fatty acid monoglyceryl esters and amides. These new derivatives were found to have potent growth inhibition effects against A549 lung cancer cells.

  5. One-Pot Synthesis of 7-Hydroxy-3-Carboxycoumarin in Water

    ERIC Educational Resources Information Center

    Fringuelli, Francesco; Piermatti, Oriana; Pizzo, Ferdinando

    2004-01-01

    The preparation of 7-hydroxy-3-carboxycoumarin starting from 2,4-dihydroxybenzaldehyde, and malonitrile, by one-pot consecutive reactions, carried out in water under heterogenous conditions is presented. The experiment encourages students to think in terms of reaction mechanisms.

  6. Synthesis of 2-aminoquinoline-3-carboamides and pyrimido[4,5-b]quinolin-4-ones through copper-catalyzed one-pot multicomponent reactions.

    PubMed

    Zhang, Xin-Ying; Guo, Xiao-Jie; Fan, Xue-Sen

    2015-01-01

    Pyrimido[4,5-b]quinolinones have attracted considerable interest from both chemical and medicinal scientists as these compounds display remarkable antimicrobial, anti-inflammatory, antitumor, antiallergy, analgesic, and antioxidant activities. The importance of pyrimido[4,5-b]quinolinones has stimulated enormous efforts to develop efficient methodologies for their synthesis. Herein, we disclose a novel synthetic protocol toward pyrimido[4,5-b]quinolin-4-ones through Cu(OAc)2 -catalyzed one-pot four-component reactions of 2-bromobenzaldehydes, aqueous ammonia, cyanoacetamides and aldehydes. The synthetic procedure combines amination/condensation/cyclization/dehydrogenation reactions in one pot, allowing synthesis of complex compounds in a simple and practical manner. Compared with literature procedures, the synthetic strategies developed herein showed advantages such as readily available and economically sustainable starting materials, structural diversity of products, good functional group tolerance, and a remarkably simple operation process. PMID:25318983

  7. BF₃·OEt₂ mediated metal-free one-pot sequential multiple annulation cascade (SMAC) synthesis of complex and diverse tetrahydroisoquinoline fused hybrid molecules.

    PubMed

    Shinde, Anand H; Vidyacharan, Shinde; Sharada, Duddu S

    2016-03-28

    A highly efficient and distinct BF3·OEt2 mediated metal-free SMAC protocol for the synthesis of complex and diverse hybrid molecules viz. indazole fused tetrahydroisoquinolinoquinoxalines, and tetrahydroisoquinolinodiazepine has been developed. The transformation is based on sequential cascade processes involving 2H-indazole formation and deprotection Pictet-Spengler cyclization steps in one-pot fashion. The protocol demonstrates the utility of sequential multiple annulations in a cascade fashion. The present one-pot protocol uses the Solid State Melt Reaction (SSMR) strategy for the synthesis of the intermediate 2H-indazole. The method is operationally simple and represents a new approach for C-C, three C-N and N-N bond formation with a wide substrate scope. PMID:26935814

  8. One-pot synthesis of yolk-shell materials with single, binary, ternary, quaternary, and quinary systems.

    PubMed

    Hong, Young Jun; Son, Mun Yeong; Park, Byung Kyu; Kang, Yun Chan

    2013-07-01

    A facile, one-pot method of systematically synthesizing yolk-shell materials with complex compositions is proposed. The spray pyrolysis process for obtaining yolk-shell materials is advantageous because it is highly efficient, allows high throughput, comprises a single-step reaction, and is a continuous process that yields homogeneous composition and enables facile control of the mean size.

  9. Praseodymium methanesulfonate catalyzed one-pot synthesis of 3,4-dihydropyrimidin-2-(1H)-ones.

    PubMed

    Wang, Min; Song, Zhiguo; Gong, Hong; Jiang, Heng

    2008-01-01

    A series of 3,4-dihydropyrimidin-2-(1H)-ones compounds was synthesized efficiently by a one-pot cyclocondensation of an aldehyde, 1,3-dicarbonyl compound, and urea in absolute ethanol under refluxing temperature using praseodymium methanesulfonate as catalyst. After the reaction, the catalyst can be easily recovered and reused several times without distinct decrease in reaction yields.

  10. One-pot, green synthesis of gold nanoparticles by gelatin and investigation of their biological effects on Osteoblast cells.

    PubMed

    Suarasan, Sorina; Focsan, Monica; Soritau, Olga; Maniu, Dana; Astilean, Simion

    2015-08-01

    It is useful to find new methods to synthesize and, more importantly, to control the size and shape of gold nanoparticles (AuNPs) without using relatively toxic-reducing agents and surfactants. In this work, we present a one-pot, green synthesis of AuNPs taking the advantage of gelatin biopolymer to operate as unique reducing, growth controlling and stabilizing agent in aqueous solution of tetrachloroauric acid (HAuCl4) at temperatures above its melting point (∼35°C). The shape and size of AuNPs were found to be strongly influenced by the gelatin concentration (0.5-5%), while the growth rate of AuNPs is controlled by temperature of synthesis (40-80°C) and viscosity of the biopolymer. A specific class of gelatin-coated AuNPs was selected to investigate its stability in simulated physiological conditions and cellular media and subsequently to evaluate the in vitro biocompatibility and capacity to sustain proliferation and differentiation of Osteoblast cells. Dark-field microscopy and Rayleigh scattering spectra prove a more efficient internalization of gelatin-coated AuNPs as compared with citrate-coated AuNPs, while methylthiazoltetrazolium bromide (MTT) assay demonstrates enhanced cell proliferation. Interestingly, in the presence of gelatin-coated AuNPs, we find out a first sign of Osteoblast cells differentiation with bone nodules formation, as confirmed by alkaline phosphatase (ALP) activity assay.

  11. One-pot synthesis of carbon-supported dendritic Pd-Au nanoalloys for electrocatalytic ethanol oxidation.

    PubMed

    Kang, Shin Wook; Lee, Young Wook; Kim, Minjung; Hong, Jong Wook; Han, Sang Woo

    2011-03-01

    One-pot synthesis of carbon-supported Pd-Au alloy nanoparticles with well-defined dendritic shape (Pd-Au(den)/C) was achieved by co-reduction of K(2)PdCl(4)/HAuCl(4) mixtures in a molar ratio of 1:1 with hydrazine in the presence of Vulcan XC-72R. The prepared Pd-Au(den)/C exhibited significantly enhanced performance in the electrocatalytic oxidation of ethanol compared with dendritic Pd nanoparticles and a commercial Pd/C catalyst. Pd-Au(den)/C even showed higher durability in electro-oxidation of ethanol than the supported catalyst prepared by the deposition of presynthesized dendritic Pd-Au nanoparticles on the carbon support. The experimental results clearly indicate that enhanced interaction between nanoparticle catalysts and carbon support through the one-pot synthesis protocol can improve the durability of the electrocatalysts.

  12. One-pot synthesis, encapsulation, and solubilization of size-tuned quantum dots with amphiphilic multidentate ligands.

    PubMed

    Kairdolf, Brad A; Smith, Andrew M; Nie, Shuming

    2008-10-01

    We report one-pot synthesis, encapsulation, and solubilization of high-quality quantum dots (QDs) based on the use of amphiphilic and multidentate polymer ligands. In this "all-in-one" procedure, the resulting QDs are first capped by the multidentate ligand and are then spontaneously encapsulated and solubilized by a second layer of the same multidentate polymer upon exposure to water. In addition to providing better control of nanocrystal nucleation and growth kinetics (including resistance to Ostwald ripening), this procedure allows for in situ growth of an inorganic passivating shell on the nanocrystal core, enabling one-pot synthesis of both type-I and type-II core-shell QDs with tunable light emission from visible to near-infrared wavelengths.

  13. One-Pot Ketone Synthesis with Alkylzinc Halides Prepared from Alkyl Halides via a Single Electron Transfer (SET) Process: New Extension of Fukuyama Ketone Synthesis.

    PubMed

    Lee, Jung Hwa; Kishi, Yoshito

    2016-06-01

    One-pot ketone synthesis has been developed with in situ activation of alkyl halides to alkylzinc halides in the presence of thioesters and Pd-catalyst. The new method provides us with a reliable option for a coupling at a late stage in a convergent synthesis of complex molecules, with use of a near 1:1 molar ratio of coupling partners. First, two facile, orthogonal methods have been developed for preparation of alkylzinc halides: (1) direct insertion of zinc dust to 1°- and 2°-alkyl halides in the presence of LiI in DMI and (2) early transition-metal assisted activation of alkyl halides via a single electron transfer (SET) process. CrCl2 has been found as an unprecedented, inevitable mediator for preparation of alkylzinc halides from alkyl halides, where CrCl2 likely functions to trap R·, generated via a SET process, and transfer it to Zn(II) to form RZnX. In addition to a commonly used CoPc, a new radical initiator NbCpCl4 has been discovered through the study. Second, with use of the two orthogonal methods, three sets of coupling conditions have been developed to complete one-pot ketone synthesis, with Condition A (Pd2dba3, PR3, Zn, LiI, TESCl, DMI), Condition B (A + CrCl2), and Condition C (B + NbCpCl4 or CoPc) being useful for simple linear and α-substituted substrates, simple linear and β-substituted substrates, and complex substrates, respectively. Condition C is applicable to the broadest range of substrates. Overall, one-pot ketone synthesis gives excellent yields, with good functional group tolerance. Controlled formation of alkylzinc halides by a combination of CrCl2 and NbCpCl4 or CoPc is crucial for its application to complex substrates. Interestingly, one-pot ketone synthesis does not suffer from the chemical instability due to the inevitable radical pathway(s), for example a 1,5-H shift. Notably, even with the increase in molecular size, no significant decrease in coupling efficiency has been noticed. To illustrate the synthetic value at a late

  14. Sequential decarboxylative azide-alkyne cycloaddition and dehydrogenative coupling reactions: one-pot synthesis of polycyclic fused triazoles.

    PubMed

    Bharathimohan, Kuppusamy; Ponpandian, Thanasekaran; Ahamed, A Jafar; Bhuvanesh, Nattamai

    2014-01-01

    Herein, we describe a one-pot protocol for the synthesis of a novel series of polycyclic triazole derivatives. Transition metal-catalyzed decarboxylative CuAAC and dehydrogenative cross coupling reactions are combined in a single flask and achieved good yields of the respective triazoles (up to 97% yield). This methodology is more convenient to produce the complex polycyclic molecules in a simple way.

  15. One-pot two-step synthesis of core-shell mesoporous silica-coated gold nanoparticles.

    PubMed

    Song, Ji-Tao; Zhang, Xiao-Shuai; Qin, Meng-Yao; Zhao, Yuan-Di

    2015-05-01

    Gold nanoparticles coated with mesoporous silica (Au@mSiO2) have been prepared by a facile one-pot two-step method. The resultant Au@mSiO2 exhibit an ideal core-shell structure with uniform mSiO2 coverage and without any interfacial adhesive layer on the Au surface. Some new explanations on the role that CTAB plays in the synthesis of Au@mSiO2 are discussed.

  16. One-pot synthesis of indenonaphthopyrans catalyzed by copper(II) triflate: a comparative study of reflux and ultrasound methods.

    PubMed

    Turhan, Kadir; Ozturkcan, S Arda; Uluer, Mehmet; Turgut, Zuhal

    2014-01-01

    An effective and environment-friendly protocol for the synthesis of indenonaphthopyrans has been developed by one-pot reaction of 2-naphthol, various aromatic aldehydes and 1,3-indandione, in the presence of copper(II) triflate as the catalyst while using reflux (Method A) and ultrasound (Method B). The Method B approach offers the advantages of a simple reaction method, short reaction time, excellent yield, and showcases the economic importance of the catalysts for such processes. PMID:25286219

  17. Sequential decarboxylative azide–alkyne cycloaddition and dehydrogenative coupling reactions: one-pot synthesis of polycyclic fused triazoles

    PubMed Central

    Bharathimohan, Kuppusamy; Ponpandian, Thanasekaran; Bhuvanesh, Nattamai

    2014-01-01

    Summary Herein, we describe a one-pot protocol for the synthesis of a novel series of polycyclic triazole derivatives. Transition metal-catalyzed decarboxylative CuAAC and dehydrogenative cross coupling reactions are combined in a single flask and achieved good yields of the respective triazoles (up to 97% yield). This methodology is more convenient to produce the complex polycyclic molecules in a simple way. PMID:25670973

  18. Sequential decarboxylative azide-alkyne cycloaddition and dehydrogenative coupling reactions: one-pot synthesis of polycyclic fused triazoles.

    PubMed

    Bharathimohan, Kuppusamy; Ponpandian, Thanasekaran; Ahamed, A Jafar; Bhuvanesh, Nattamai

    2014-01-01

    Herein, we describe a one-pot protocol for the synthesis of a novel series of polycyclic triazole derivatives. Transition metal-catalyzed decarboxylative CuAAC and dehydrogenative cross coupling reactions are combined in a single flask and achieved good yields of the respective triazoles (up to 97% yield). This methodology is more convenient to produce the complex polycyclic molecules in a simple way. PMID:25670973

  19. Domino [Pd]-Catalysis: One-Pot Synthesis of Isobenzofuran-1(3H)-ones.

    PubMed

    Mahendar, Lodi; Satyanarayana, Gedu

    2016-09-01

    An efficient domino [Pd]-catalysis for the synthesis of isobenzofuran-1(3H)-ones is presented. The strategy shows broad substrate scope and is amenable to o-bromobenzyl tertiary/secondary/primary alcohols. Significantly, the method was applied to the synthesis of antiplatelet drug n-butyl phthalide and cytotoxic agonist 3a-[4'-methoxylbenzyl]-5,7-dimethoxyphthalide. PMID:27509096

  20. A one-pot synthesis of α-l-threofuranosyl nucleoside triphosphates (tNTPs).

    PubMed

    Sau, Sujay P; Chaput, John C

    2016-07-15

    TNA (α-l-threofuranosyl nucleoside) triphosphates of adenosine (tATP), guanosine (tGTP), cytidine (tCTP), and thymidine (tTTP) were synthesized from their corresponding 3'-O-phosphoramidite derivatives using a novel one-pot reaction that is less moisture sensitive than traditional methods. The chemically synthesized tNTPs, despite containing an unnatural 3'-triphosphate moiety, are similar in thermal stability to natural nucleotide triphosphates. PMID:27246616

  1. One-pot synthesis and characterization of subnanometre-size benzotriazolate protected copper clusters.

    PubMed

    Salorinne, Kirsi; Chen, Xi; Troff, Ralf W; Nissinen, Maija; Häkkinen, Hannu

    2012-07-21

    A simple one-pot method for the preparation of subnanometre-size benzotriazolate (BTA) protected copper clusters, Cu(n)BTA(m), is reported. The clusters were analyzed by optical and infrared spectroscopy, mass spectrometry and transmission electron microscopy together with computational methods. We suggest a structural motif where the copper core of the Cu(n)BTA(m) clusters is protected by BTA-Cu(i)-BTA units.

  2. One-Pot Synthesis of Substituted Trifluoromethylated 2,3-Dihydro-1H-imidazoles.

    PubMed

    Deutsch, Amrei; Jessen, Christoph; Deutsch, Carl; Karaghiosoff, Konstantin; Hoffmann-Röder, Anja

    2016-07-15

    An operationally simple one-pot reaction for the preparation of a novel class of racemic trifluoromethylated 2,3-dihydro-1H-imidazoles derived from electron-poor N,O-acetals and aryl Grignard reagents is described. In addition, access to highly functionalized 2-trifluoromethyl-2,3-dihydro-1H-imidazoles was accomplished by reaction of N-aryl hemiaminal ethers and N-aryl trifluoroethylamines in the presence of an excess of n-butyllithium. PMID:27359260

  3. One-pot synthesis, photoluminescence, and electrocatalytic properties of subnanometer-sized copper clusters.

    PubMed

    Wei, Wentao; Lu, Yizhong; Chen, Wei; Chen, Shaowei

    2011-02-23

    Subnanometer-sized copper nanoclusters were prepared by a one-pot procedure based on wet chemical reduction. The structural characteristics of the 2-mercapto-5-n-propylpyrimidine-protected nanoclusters, Cu(n) (n ≤ 8), were determined by mass spectrometry. The Cu nanoclusters displayed apparent luminescence, with dual emissions at 425 and 593 nm, with quantum yields of 3.5 and 0.9%, respectively, and high electrocatalytic activity in the electoreduction of oxygen.

  4. One-pot gold-catalyzed synthesis of 3-silylethynyl indoles from unprotected o-alkynylanilines

    PubMed Central

    Brand, Jonathan P; Chevalley, Clara

    2011-01-01

    Summary The Au(III)-catalyzed cyclization of 2-alkynylanilines was combined in a one-pot procedure with the Au(I)-catalyzed C3-selective direct alkynylation of indoles using the benziodoxolone reagent TIPS-EBX to give a mild, easy and straightforward entry to 2-substituted-3-alkynylindoles. The reaction can be applied to unprotected anilines, was tolerant to functional groups and easy to carry out (RT, and requires neither an inert atmosphere nor special solvents). PMID:21647264

  5. A one-pot synthesis of α-l-threofuranosyl nucleoside triphosphates (tNTPs).

    PubMed

    Sau, Sujay P; Chaput, John C

    2016-07-15

    TNA (α-l-threofuranosyl nucleoside) triphosphates of adenosine (tATP), guanosine (tGTP), cytidine (tCTP), and thymidine (tTTP) were synthesized from their corresponding 3'-O-phosphoramidite derivatives using a novel one-pot reaction that is less moisture sensitive than traditional methods. The chemically synthesized tNTPs, despite containing an unnatural 3'-triphosphate moiety, are similar in thermal stability to natural nucleotide triphosphates.

  6. A quadruple cascade protocol for the one-pot synthesis of fully-substituted hexahydroisoindolinones from simple substrates.

    PubMed

    Zhang, Hong-Bo; Luo, Yong-Chun; Hu, Xiu-Qin; Liang, Yong-Min; Xu, Peng-Fei

    2016-01-01

    A new and efficient synthetic method to obtain fully-substituted hexahydroisoindolinones was developed by using bifunctional tertiary amine-thioureas as powerful catalysts. As far as we know, there is no efficient synthetic method developed toward fully-substituted hexahydroisoindolinones. The products were obtained in good yield and diastereoselectivity. The one-pot cascade quadruple protocol features readily available starting materials, simple manipulation, mild conditions and good atom economy.

  7. One-pot solvothermal synthesis of highly water-dispersible size-tunable functionalized magnetite nanocrystal clusters for lipase immobilization.

    PubMed

    Zhu, Hao; Hou, Chen; Li, Yijing; Zhao, Guanghui; Liu, Xiao; Hou, Ke; Li, Yanfeng

    2013-07-01

    A facile one-pot synthesis of highly water-dispersible size-tunable magnetite (Fe3O4) nanocrystal clusters (MNCs) end-functionalized with amino or carboxyl groups by a modified solvothermal reduction reaction has been developed. Dopamine and 3,4-dihydroxyhydroxycinnamic acid were used for the first time as both a surfactant and interparticle linker in a polylol process for economical and environment-friendly purposes. Morphology, chemical composition, and magnetic properties of the prepared particles were investigated by several methods, including FESEM, TEM, XRD, XPS, Raman, FTIR, TGA, zeta potential, and VSM. The sizes of the particles could be easily tuned over a wide range from 175 to 500 nm by varying the surfactant concentration. Moreover, ethylene glycol/diethylene glycol (EG/DEG) solvent mixtures with different ratios could be used as reductants to obtain the particles with smaller sizes. The XRD data demonstrated that the surfactants restrained the crystal growth of the grains. The nanoparticles showed superior magnetic properties and high colloidal stability in water. The cytotoxicity results indicated the feasibility of using the synthesized nanocrystals in biology-related fields. To estimate the applicability of the obtained MNCs in biotechnology, Candida rugosa lipase was selected for the enzyme immobilization process. The immobilized lipase exhibited excellent thermal stability and reusability in comparison with the free enzyme. This novel strategy would simplify the reaction protocol and improve the efficiency of materials functionalization, thus offering new potential applications in biotechnology and organocatalysis.

  8. One-Pot Synthesis of SnO2/C Nanocapsules Composites as Anode Materials for Lithium-Ion Batteries.

    PubMed

    Yang, Lina; Chen, Kexun; Dong, Tao; Wang, Zhao; Li, Guomin; Zhang, Yanling; Zhang, Lipeng

    2016-02-01

    In this work, we demonstrate a facile route for the synthesis of nanostructured SnO2/C composites for lithium-ion batteries. The anode materials were prepared via a one-pot solvothermal approach and then calcination in a highly pure nitrogen atmosphere. The composited was composed of amor- phous carbon and nanocrystalline SnO2 by the X-ray diffraction (XRD) analysis, and the content of carbon was calculated according to the thermogravimetric analysis (TGA). Scanning electron microscopy (SEM) images revealed that the diameter of these as-prepared spheres varied from 50 to 60 nm. A systematic study has been carried out to examine the effect of carbon content upon lithium-ion battery performance. The electrochemical results showed that SnO2/C nanocomposite could achieve 1197.5 mAh/g reversible capacity and 55.11% initial coulombic efficiency, and 190% capacity retention after 50 cycles compared to the SnO2 nanoparticles of 940.6 mAh/g at a current density 0.2 C in the voltage range of 0.01-3.0 V. These improvements can be ascribed to the carbon, which can enhance the conductivity of SnO2, suppress the aggregation of active particles, and increase their structural stability during cycling. PMID:27433668

  9. One-pot hydrothermal synthesis of zeolite/sodium tantalate composite and its photodegradation of methyl orange

    SciTech Connect

    Gu, Xiaoli; Lu, Haiqiang; Kan, Chun; Yao, Jianfeng

    2015-08-15

    Highlights: • Sodalite/NaTaO{sub 3} composite is prepared by a one-pot hydrothermal synthesis. • Enhanced photodegradation is achieved due to the heterogeneous doping effect. • Structure distortion is found for NaTaO{sub 3} after removing sodalite by acid washing. - Abstract: Sodalite/NaTaO{sub 3} composite was prepared by a one-pot hydrothermal synthesis method. Sodalite and NaTaO{sub 3} grow interpenetrated, and the resulting composites have similar morphology as the pure sodalite. The sodalite/NaTaO{sub 3} composite has a lower band gap of 3.35 eV due to the heterogeneous doping effect, and exhibits an enhanced photodegradation of methyl orange under UV irradiation as compared to the pure NaTaO{sub 3}. A slight structure distortion is found for NaTaO{sub 3} after removing sodalite by acid washing the sodalite/NaTaO{sub 3} composite, and such result further confirms the co-growth of the two crystals. This one-pot hydrothermal method opens up new avenues for the preparation of photocatalytic composites.

  10. Effect of amine addition on the synthesis of CdSe nanocrystals in liquid paraffin via one-pot method

    NASA Astrophysics Data System (ADS)

    Jia, Jinqian; Tian, Jintao; Tian, Weiguo; Mi, Wen; Liu, Xiaoyun; Dai, Jinhui; Wang, Xin

    2014-02-01

    The effect of n-octylamine (OA) and octadecylamine (ODA) addition on the synthesis of CdSe nanocrystals in liquid paraffin via one-pot method is investigated via the measurements of their ultraviolet-visible absorption and fluorescence emission spectra. Our results showed that the in situ added amines can activate the formation reaction of Cd precursor and, as a result, substantially decrease the initial reaction temperature and accelerate the particle growth. By adding OA at high temperature of 200 °C, remarkable improvement on particle quality is achieved, giving relatively narrow size distribution of 33.1 nm and high photoluminescence quantum yield (PLQY) of 81.9% for the CdSe nanoparticles. OA addition at low temperature shows also good quality improvement for the nanoparticles. With regard to the primary amine of ODA, it may be inappropriate for quality improvement of the CdSe nanoparticles from liquid paraffin via one-pot method.

  11. One-pot synthesis of enantiomerically pure N-protected allylic amines from N-protected α-amino esters

    PubMed Central

    Silveira-Dorta, Gastón; Álvarez-Méndez, Sergio J; Martín, Víctor S

    2016-01-01

    Summary An improved protocol for the synthesis of enantiomerically pure allylic amines is reported. N-Protected α-amino esters derived from natural amino acids were submitted to a one-pot tandem reduction–olefination process. The sequential reduction with DIBAL-H at −78 °C and subsequent in situ addition of organophosphorus reagents yielded the corresponding allylic amines without the need to isolate the intermediate aldehyde. This circumvents the problem of instability of the aldehydes. The method tolerates well both Wittig and Horner–Wadsworth–Emmons organophosphorus reagents. A better Z-(dia)stereoselectivity was observed when compared to the previous one-pot method. The (dia)stereoselectivity of the process was affected neither by the reaction solvent nor by the amount of DIBAL-H employed. The method is compatible with the presence of free hydroxy groups as shown with serine and threonine derivatives. PMID:27340486

  12. One-pot synthesis of enantiomerically pure N-protected allylic amines from N-protected α-amino esters.

    PubMed

    Silveira-Dorta, Gastón; Álvarez-Méndez, Sergio J; Martín, Víctor S; Padrón, José M

    2016-01-01

    An improved protocol for the synthesis of enantiomerically pure allylic amines is reported. N-Protected α-amino esters derived from natural amino acids were submitted to a one-pot tandem reduction-olefination process. The sequential reduction with DIBAL-H at -78 °C and subsequent in situ addition of organophosphorus reagents yielded the corresponding allylic amines without the need to isolate the intermediate aldehyde. This circumvents the problem of instability of the aldehydes. The method tolerates well both Wittig and Horner-Wadsworth-Emmons organophosphorus reagents. A better Z-(dia)stereoselectivity was observed when compared to the previous one-pot method. The (dia)stereoselectivity of the process was affected neither by the reaction solvent nor by the amount of DIBAL-H employed. The method is compatible with the presence of free hydroxy groups as shown with serine and threonine derivatives. PMID:27340486

  13. An Electron-Poor C64 Nanographene by Palladium-Catalyzed Cascade C-C Bond Formation: One-Pot Synthesis and Single-Crystal Structure Analysis.

    PubMed

    Seifert, Sabine; Shoyama, Kazutaka; Schmidt, David; Würthner, Frank

    2016-05-23

    Herein, we report the one-pot synthesis of an electron-poor nanographene containing dicarboximide groups at the corners. We efficiently combined palladium-catalyzed Suzuki-Miyaura cross-coupling and dehydrohalogenation to synthesize an extended two-dimensional π-scaffold of defined size in a single chemical operation starting from N-(2,6-diisopropylphenyl)-4,5-dibromo-1,8-naphthalimide and a tetrasubstituted pyrene boronic acid ester as readily accessible starting materials. The reaction of these precursors under the conditions commonly used for Suzuki-Miyaura cross-coupling afforded a C64 nanographene through the formation of ten C-C bonds in a one-pot process. Single-crystal X-ray analysis unequivocally confirmed the structure of this unique extended aromatic molecule with a planar geometry. The optical and electrochemical properties of this largest ever synthesized planar electron-poor nanographene skeleton were also analyzed.

  14. Pseudo five-component synthesis of 2,5-di(hetero)arylthiophenes via a one-pot Sonogashira-Glaser cyclization sequence.

    PubMed

    Urselmann, Dominik; Antovic, Dragutin; Müller, Thomas J J

    2011-01-01

    Based upon a consecutive one-pot Sonogashira-Glaser coupling-cyclization sequence a variety of 2,5-di(hetero)arylthiophenes were synthesized in moderate to good yields. A single Pd/Cu-catalyst system, without further catalyst addition, and easily available, stable starting materials were used, resulting in a concise and highly efficient route for the synthesis of the title compounds. This novel pseudo five-component synthesis starting from iodo(hetero)arenes is particularly suitable as a direct access to well-defined thiophene oligomers, which are of peculiar interest in materials science. PMID:22238523

  15. Pseudo five-component synthesis of 2,5-di(hetero)arylthiophenes via a one-pot Sonogashira–Glaser cyclization sequence

    PubMed Central

    Urselmann, Dominik; Antovic, Dragutin

    2011-01-01

    Summary Based upon a consecutive one-pot Sonogashira–Glaser coupling–cyclization sequence a variety of 2,5-di(hetero)arylthiophenes were synthesized in moderate to good yields. A single Pd/Cu-catalyst system, without further catalyst addition, and easily available, stable starting materials were used, resulting in a concise and highly efficient route for the synthesis of the title compounds. This novel pseudo five-component synthesis starting from iodo(hetero)arenes is particularly suitable as a direct access to well-defined thiophene oligomers, which are of peculiar interest in materials science. PMID:22238523

  16. One-pot palladium-catalyzed borrowing hydrogen synthesis of thioethers.

    PubMed

    Corma, Avelino; Navas, Javier; Ródenas, Tania; Sabater, María J

    2013-12-16

    Palladium on magnesium oxide is able to allow a one-pot reaction to synthesize thioethers from thiols and aldehydes formed in situ from the respective alcohol by means of a borrowing hydrogen method. The reaction is initiated by dehydrogenation of the alcohol to give a palladium hydride intermediate and an aldehyde. The latter reacts with a thiol involving most probably the intermediacy of a thionium ion RCH=S(+)R, which can be reduced in situ by the metal hydride to afford thioethers. PMID:24259460

  17. Concise synthesis of complicated polypropionates through one-pot dissymmetrical two-directional chain elongation.

    PubMed

    Exner, Claudia J; Turks, Maris; Fonquerne, Freddy; Vogel, Pierre

    2011-04-01

    Herein, a major breakthrough in a sulfur dioxide-mediated oxyallylation cascade reaction is reported that allows the preparation of complex long-chain polyketide fragments with more than ten stereogenic centers through a carefully designed desymmetrization process. An allylbissilane is combined, under the appropriate reaction conditions, with two different 1,3-dioxy-1,3-dienes permitting the construction of a 13-membered polypropionate precursor in one pot. Four stereocenters are selectively created during this process. The so-obtained pseudo-C(2)- or -C(S)-symmetric products are desymmetrized through selective deprotection and can be selectively elongated in both directions using aldol chemistry.

  18. One-pot synthesis of Bi-Ni nanowire and nanocable arrays by coelectrodeposition approach

    PubMed Central

    2012-01-01

    A novel and convenient one-pot electrodeposition approach has been developed for precisely controlled fabrication of large-scale Bi-Ni nanowire and nanocable arrays. Using porous anodic aluminum oxide as a shape-directing template, by simply changing the electrochemical deposition mode, desired Bi-Ni hybrid nanowires and Bi-Ni core-shell nanocables have been obtained in the CV and CC modes, respectively. The structure, morphology, and composition of the as-prepared samples were characterized using X-ray powder diffraction, transmission electron microscopy, elemental mapping, and energy-dispersive X-ray spectrometry. PMID:22336749

  19. Size-tunable polymeric nanoreactors for one-pot synthesis and encapsulation of quantum dots.

    PubMed

    Qian, Guannan; Zhu, Benchuan; Wang, Youfu; Deng, Sheng; Hu, Aiguo

    2012-08-28

    Hydrophilic polymeric nanoparticles are synthesized through a Bergman cyclization- mediated intramolecular chain collapse of structurally well-defined linear polymers, and then used as size-tunable nanoreactors to fabricate and encapsulate quantum dots in a one-pot reaction. Crystalline quantum dots are formed in all of these nanoreactors and visualized by transmission electron microscopy. Smaller nanoreactors produce one quantum dot each while larger nanoreactors form a number, resulting in fluorescence quenching. By controlling the molecular weight of the linear polymer precursor, a variable number of nanocrystals are fabricated and assembled in a single nanoreactor.

  20. One-pot synthesis of β-acetamido ketones using boric acid at room temperature.

    PubMed

    Karimi-Jaberi, Zahed; Mohammadi, Korosh

    2012-01-01

    β-acetamido ketones were synthesized in excellent yields through one-pot condensation reaction of aldehydes, acetophenones, acetyl chloride, and acetonitrile in the presence of boric acid as a solid heterogeneous catalyst at room temperature. It is the first successful report of boric acid that has been used as solid acid catalyst for the preparation of β-acetamido ketones. The remarkable advantages offered by this method are green catalyst, mild reaction conditions, simple procedure, short reaction times, and good-to-excellent yields of products.

  1. One-pot synthesis of hematite@graphene core@shell nanostructures for superior lithium storage.

    PubMed

    Chen, Dezhi; Quan, Hongying; Liang, Junfei; Guo, Lin

    2013-10-21

    Novel hematite@graphene composites have been successfully synthesized by a one-pot surfactant governed approach under mild wet-chemical conditions. A series of characterizations including X-ray diffraction (XRD), Raman spectrum, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated that the hematite nanoparticles with relatively uniform size were encapsulated by graphene layers and were able to form core-shell nanostructures. The electrochemical properties of hematite@graphene core-shell nanostructures as anodes for lithium-ion batteries were evaluated by galvanostatic charge-discharge and AC impedance spectroscopy techniques. The as-prepared hematite@graphene core-shell nanostructures exhibited a high reversible specific capacity of 1040 mA h g(-1) at a current density of 200 mA g(-1) (0.2 C) after 180 cycles and excellent rate capability and long cycle life. Furthermore, a reversible capacity as high as 500 mA h g(-1) was still achieved after 200 cycles even at a high rate of 6 C. The electrochemical test results show that the hematite@graphene composites prepared by the one-pot wet chemical method are promising anode materials for lithium-ion batteries.

  2. Mussel-inspired one-pot synthesis of transition metal and nitrogen co-doped carbon (M/N-C) as efficient oxygen catalysts for Zn-air batteries.

    PubMed

    Li, Bing; Chen, Ye; Ge, Xiaoming; Chai, Jianwei; Zhang, Xiao; Hor, T S Andy; Du, Guojun; Liu, Zhaolin; Zhang, Hua; Zong, Yun

    2016-03-01

    Transition metal and nitrogen co-doping into carbon is an effective approach to promote the catalytic activities towards the oxygen reduction reaction (ORR) and/or oxygen evolution reaction (OER) in the resultant electrocatalysts, M/N-C. The preparation of such catalysts, however, is often complicated and in low yield. Herein we report a robust approach for easy synthesis of M/N-C hybrids in high yield, which includes a mussel-inspired polymerization reaction at room temperature and a subsequent carbonization process. With the introduction of selected transition metal salts into an aqueous solution of dopamine (DA), the obtained mixture self-polymerizes to form metal-containing polydopamine (M-PDA) composites, e.g. Co-PDA, Ni-PDA and Fe-PDA. Upon carbonization at elevated temperatures, these metal-containing composites were converted into M/N-C, i.e. Co-PDA-C, Ni-PDA-C and Fe-PDA-C, respectively, whose morphologies, chemical compositions, and electrochemical performances were fully studied. Enhanced ORR activities were found in all the obtained hybrids, with Co-PDA-C standing out as the most promising catalyst with excellent stability and catalytic activities towards both ORR and OER. This was further proven in Zn-air batteries (ZnABs) in terms of discharge voltage stability and cycling performance. At a discharge-charge current density of 2 mA cm(-2) and 1 h per cycle, the Co-PDA-C based ZnABs were able to steadily cycle up to 500 cycles with only a small increase in the discharge-charge voltage gap which notably outperformed Pt/C; at a discharge current density of 5 mA cm(-2), the battery continuously discharged for more than 540 h with the discharge voltage above 1 V and a voltage drop rate of merely 0.37 mV h(-1). With the simplicity and scalability of the synthetic approach and remarkable battery performances, the Co-PDA-C hybrid catalyst is anticipated to play an important role in practical ZnABs.

  3. Mussel-inspired one-pot synthesis of transition metal and nitrogen co-doped carbon (M/N-C) as efficient oxygen catalysts for Zn-air batteries.

    PubMed

    Li, Bing; Chen, Ye; Ge, Xiaoming; Chai, Jianwei; Zhang, Xiao; Hor, T S Andy; Du, Guojun; Liu, Zhaolin; Zhang, Hua; Zong, Yun

    2016-03-01

    Transition metal and nitrogen co-doping into carbon is an effective approach to promote the catalytic activities towards the oxygen reduction reaction (ORR) and/or oxygen evolution reaction (OER) in the resultant electrocatalysts, M/N-C. The preparation of such catalysts, however, is often complicated and in low yield. Herein we report a robust approach for easy synthesis of M/N-C hybrids in high yield, which includes a mussel-inspired polymerization reaction at room temperature and a subsequent carbonization process. With the introduction of selected transition metal salts into an aqueous solution of dopamine (DA), the obtained mixture self-polymerizes to form metal-containing polydopamine (M-PDA) composites, e.g. Co-PDA, Ni-PDA and Fe-PDA. Upon carbonization at elevated temperatures, these metal-containing composites were converted into M/N-C, i.e. Co-PDA-C, Ni-PDA-C and Fe-PDA-C, respectively, whose morphologies, chemical compositions, and electrochemical performances were fully studied. Enhanced ORR activities were found in all the obtained hybrids, with Co-PDA-C standing out as the most promising catalyst with excellent stability and catalytic activities towards both ORR and OER. This was further proven in Zn-air batteries (ZnABs) in terms of discharge voltage stability and cycling performance. At a discharge-charge current density of 2 mA cm(-2) and 1 h per cycle, the Co-PDA-C based ZnABs were able to steadily cycle up to 500 cycles with only a small increase in the discharge-charge voltage gap which notably outperformed Pt/C; at a discharge current density of 5 mA cm(-2), the battery continuously discharged for more than 540 h with the discharge voltage above 1 V and a voltage drop rate of merely 0.37 mV h(-1). With the simplicity and scalability of the synthetic approach and remarkable battery performances, the Co-PDA-C hybrid catalyst is anticipated to play an important role in practical ZnABs. PMID:26864616

  4. Mussel-inspired one-pot synthesis of transition metal and nitrogen co-doped carbon (M/N-C) as efficient oxygen catalysts for Zn-air batteries

    NASA Astrophysics Data System (ADS)

    Li, Bing; Chen, Ye; Ge, Xiaoming; Chai, Jianwei; Zhang, Xiao; Hor, T. S. Andy; Du, Guojun; Liu, Zhaolin; Zhang, Hua; Zong, Yun

    2016-02-01

    Transition metal and nitrogen co-doping into carbon is an effective approach to promote the catalytic activities towards the oxygen reduction reaction (ORR) and/or oxygen evolution reaction (OER) in the resultant electrocatalysts, M/N-C. The preparation of such catalysts, however, is often complicated and in low yield. Herein we report a robust approach for easy synthesis of M/N-C hybrids in high yield, which includes a mussel-inspired polymerization reaction at room temperature and a subsequent carbonization process. With the introduction of selected transition metal salts into an aqueous solution of dopamine (DA), the obtained mixture self-polymerizes to form metal-containing polydopamine (M-PDA) composites, e.g. Co-PDA, Ni-PDA and Fe-PDA. Upon carbonization at elevated temperatures, these metal-containing composites were converted into M/N-C, i.e. Co-PDA-C, Ni-PDA-C and Fe-PDA-C, respectively, whose morphologies, chemical compositions, and electrochemical performances were fully studied. Enhanced ORR activities were found in all the obtained hybrids, with Co-PDA-C standing out as the most promising catalyst with excellent stability and catalytic activities towards both ORR and OER. This was further proven in Zn-air batteries (ZnABs) in terms of discharge voltage stability and cycling performance. At a discharge-charge current density of 2 mA cm-2 and 1 h per cycle, the Co-PDA-C based ZnABs were able to steadily cycle up to 500 cycles with only a small increase in the discharge-charge voltage gap which notably outperformed Pt/C; at a discharge current density of 5 mA cm-2, the battery continuously discharged for more than 540 h with the discharge voltage above 1 V and a voltage drop rate of merely 0.37 mV h-1. With the simplicity and scalability of the synthetic approach and remarkable battery performances, the Co-PDA-C hybrid catalyst is anticipated to play an important role in practical ZnABs.Transition metal and nitrogen co-doping into carbon is an effective

  5. Mussel-inspired one-pot synthesis of transition metal and nitrogen co-doped carbon (M/N-C) as efficient oxygen catalysts for Zn-air batteries

    NASA Astrophysics Data System (ADS)

    Li, Bing; Chen, Ye; Ge, Xiaoming; Chai, Jianwei; Zhang, Xiao; Hor, T. S. Andy; Du, Guojun; Liu, Zhaolin; Zhang, Hua; Zong, Yun

    2016-02-01

    Transition metal and nitrogen co-doping into carbon is an effective approach to promote the catalytic activities towards the oxygen reduction reaction (ORR) and/or oxygen evolution reaction (OER) in the resultant electrocatalysts, M/N-C. The preparation of such catalysts, however, is often complicated and in low yield. Herein we report a robust approach for easy synthesis of M/N-C hybrids in high yield, which includes a mussel-inspired polymerization reaction at room temperature and a subsequent carbonization process. With the introduction of selected transition metal salts into an aqueous solution of dopamine (DA), the obtained mixture self-polymerizes to form metal-containing polydopamine (M-PDA) composites, e.g. Co-PDA, Ni-PDA and Fe-PDA. Upon carbonization at elevated temperatures, these metal-containing composites were converted into M/N-C, i.e. Co-PDA-C, Ni-PDA-C and Fe-PDA-C, respectively, whose morphologies, chemical compositions, and electrochemical performances were fully studied. Enhanced ORR activities were found in all the obtained hybrids, with Co-PDA-C standing out as the most promising catalyst with excellent stability and catalytic activities towards both ORR and OER. This was further proven in Zn-air batteries (ZnABs) in terms of discharge voltage stability and cycling performance. At a discharge-charge current density of 2 mA cm-2 and 1 h per cycle, the Co-PDA-C based ZnABs were able to steadily cycle up to 500 cycles with only a small increase in the discharge-charge voltage gap which notably outperformed Pt/C; at a discharge current density of 5 mA cm-2, the battery continuously discharged for more than 540 h with the discharge voltage above 1 V and a voltage drop rate of merely 0.37 mV h-1. With the simplicity and scalability of the synthetic approach and remarkable battery performances, the Co-PDA-C hybrid catalyst is anticipated to play an important role in practical ZnABs.Transition metal and nitrogen co-doping into carbon is an effective

  6. Palladium-Catalyzed Benzylic Arylation of Pyridylmethyl Silyl Ethers: One-Pot Synthesis of Aryl(pyridyl)methanols.

    PubMed

    Rivero, Alexandra R; Kim, Byeong-Seon; Walsh, Patrick J

    2016-04-01

    An efficient palladium-catalyzed direct arylation of pyridylmethyl silyl ethers with aryl bromides is described. A Pd(OAc)2/NIXANTPHOS-based catalyst provides aryl(pyridyl)methyl alcohol derivatives in good to excellent yields (33 examples, 57-100% yield). This protocol is compatible with different silyl ether protecting groups, affording either the protected or the free alcohols in an effective one-pot process. The scalability of the reaction is demonstrated. PMID:27004592

  7. Au-ZnO hybrid nanoflowers, nanomultipods and nanopyramids: one-pot reaction synthesis and photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Chen, Yuanzhi; Zeng, Deqian; Zhang, Kun; Lu, Aolin; Wang, Laisen; Peng, Dong-Liang

    2013-12-01

    The preparation of noble metal-semiconductor hybrid nanocrystals with controlled morphologies has received intensive interest in recent years. In this study, facile one-pot reactions have been developed for the synthesis of Au-ZnO hybrid nanocrystals with different interesting morphologies, including petal-like and urchin-like nanoflowers, nanomultipods and nanopyramids. In the synthesis strategy, oleylamine-containing solution serves as the reaction medium, and the in situ generated Au seeds play an important role in the subsequently induced growth of ZnO nanocrystals. With the aid of several surfactants, hybrid nanocrystals with different morphologies that have considerable influences on their optical and photocatalytic activities are readily achieved. Through high-resolution transmission electron microscopy measurements, an observed common orientation relationship between ZnO and Au is that ZnO nanocrystals prefer to grow with their polar {001} facets on the {111} facets of Au nanocrystals, and well-defined interfaces are evident. Surface plasmon resonance bands of Au with different positions are observed in the UV-vis spectra, and the UV and visible emissions of ZnO are found to be dramatically reduced. Finally, the as-prepared Au-ZnO nanocrystals exhibit excellent photocatalytic activity for the photodegradation of rhodamine B compared with pure ZnO nanocrystals. The Au-ZnO hybrid nanopyramids show the highest catalytic efficiency, which is correlated with the exposed crystal facets, crystallinity and the formation of hybrid nanostructures. The as-prepared Au-ZnO hybrid nanocrystals are expected to find diverse potential applications in the fields such as photocatalysis, solar energy conversion, sensing and biological detection.The preparation of noble metal-semiconductor hybrid nanocrystals with controlled morphologies has received intensive interest in recent years. In this study, facile one-pot reactions have been developed for the synthesis of Au

  8. A New One-Pot Synthesis of Quinoline-2-carboxylates under Heterogeneous Conditions.

    PubMed

    Gabrielli, Serena; Giardinieri, Alessandra; Sampaolesi, Susanna; Ballini, Roberto; Palmieri, Alessandro

    2016-01-01

    Quinoline-2-carboxylates are an important subclass of quinoline derivatives largely present in a variety of biologically active molecules, as well as useful ligands in metal-catalyzed reactions. Herein, we present a new one-pot protocol for synthesizing this class of derivatives starting from β-nitroacrylates and 2-aminobenzaldehydes. In order to optimize the protocol, we investigated several reaction conditions, obtaining the best results using the 2-tert-Butylimino-2-diethylamino-1,3-dimethylperhydro-1,3,2-diazaphosphorine (BEMP) as solid base, in acetonitrile. Finally, we demonstrated the generality of our approach over several substrates which led to synthesize a plethora of functionalized quinolines-2-carboxylate derivatives in good overall yields.

  9. One-pot noninjection route to CdS quantum dots via hydrothermal synthesis.

    PubMed

    Aboulaich, Abdelhay; Billaud, Denis; Abyan, Mouhammad; Balan, Lavinia; Gaumet, Jean-Jacques; Medjadhi, Ghouti; Ghanbaja, Jaafar; Schneider, Raphaël

    2012-05-01

    Water-dispersible CdS quantum dots (QDs) emitting from 510 to 650 nm were synthesized in a simple one-pot noninjection hydrothermal route using cadmium chloride, thiourea, and 3-mercaptopropionic acid (MPA) as starting materials. All these chemicals were loaded at room temperature in a Teflon sealed tube and the reaction mixture heated at 100 °C. The effects of CdCl(2)/thiourea/MPA feed molar ratios, pH, and concentrations of precursors affecting the growth of the CdS QDs, was monitored via the temporal evolution of the optical properties of the CdS nanocrystals. High concentration of precursors and high MPA/Cd feed molar ratios were found to lead to an increase in the diameter of the resulting CdS nanocrystals and of the trap state emission of the dots. The combination of moderate pH value, low concentration of precursors and slow growth rate plays the crucial role in the good optical properties of the obtained CdS nanocrystals. The highest photoluminescence achieved for CdS@MPA QDs of average size 3.5 nm was 20%. As prepared colloids show rather narrow particle size distribution, although all reactants were mixed at room temperature. CdS@MPA QDs were characterized by UV-vis and photoluminescence spectroscopy, powder X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray spectrometry and MALDI TOF mass spectrometry. This noninjection one-pot approach features easy handling and large-scale production with excellent synthetic reproducibility. Surface passivation of CdS@MPA cores by a wider bandgap material, ZnS, led to enhanced luminescence intensity. CdS@MPA and CdS/ZnS@MPA QDs exhibit high photochemical stability and hold a good potential to be applied in optoelectronic devices and biological applications.

  10. Size-controlled, one-pot synthesis, characterization, and biological applications of epoxy-organosilica particles possessing positive zeta potential.

    PubMed

    Nakamura, Michihiro; Ishimura, Kazunori

    2008-11-01

    Epoxy-organosilica particles made from 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane (EpoMS) as a single silica source were synthesized by means of a one-pot method. We evaluated three sets of synthesis conditions, including traditional Stober conditions and two variations. Although the traditional conditions did not afford EpoMS particles, the variations did. The size distributions of the particles were evaluated by means of transmission electron microscopy. The mean diameters and size distributions of the particles depended on the EpoMS concentration, and the best coefficient of variation for the size distribution was 5.9%. The surface of the particles had unique properties, such as a positive zeta potential. The particles bound strongly to proteins as well as to DNA. The particles made from EpoMS, allowing particles internally functionalized with fluorescent dye to be prepared by means of a one-pot synthesis. EpoMS particles doped and tuned with fluorescent dye showed strong fluorescence signals and distinct peaks on flow cytometry, and the fluorescent particles could be used to label cells. The labeled cells showed clear fluorescence under a fluorescence microscope, and electron microscopy showed many particles in the cytoplasm. This is the first report describing the synthesis of epoxy-organosilica particles with a positive zeta potential and describing differences in the characteristics of particle formations due to changes in synthesis conditions. We also discuss the advantages of EpoMS particles, as well as the potential biological applications of these particles.

  11. Synthesis and Evaluation of Cu/SAPO-34 Catalysts for NH3-SCR 2: Solid-state Ion Exchange and One-pot Synthesis

    SciTech Connect

    Gao, Feng; Walter, Eric D.; Washton, Nancy M.; Szanyi, Janos; Peden, Charles HF

    2015-01-01

    Cu-SAPO-34 catalysts are synthesized using two methods: solid-state ion exchange (SSIE) and one-pot synthesis. SSIE is conducted by calcining SAPO-34/CuO mixtures at elevated temperatures. For the one-pot synthesis method, Cu-containing chemicals (CuO and CuSO4) are added during gel preparation. A high-temperature calcination step is also needed for this method. Catalysts are characterized with surface area/pore volume measurements, temperature programmed reduction (TPR), electron paramagnetic resonance (EPR) and nuclear magnetic resonance (NMR) spectroscopies, and scanning electron microscopy (SEM). Catalytic properties are examined using standard ammonia selective catalytic reduction (NH3-SCR) and ammonia oxidation reactions. In Cu-SAPO-34 samples formed using SSIE, Cu presents both as isolated Cu2+ ions and unreacted CuO. The former is highly active and selective in NH3-SCR, while the latter catalyzes a side reaction; notably, the non-selective oxidation of NH3 above 350 ºC. Using the one-pot method followed by a high-temperature aging treatment, it is possible to form Cu SAPO-34 samples with predominately isolated Cu2+ ions at low Cu loadings. However at much higher Cu loadings, isolated Cu2+ ions that bind weakly with the CHA framework and CuO clusters also form. These Cu moieties are very active in catalyzing non-selective NH3 oxidation above 350 ºC. Low-temperature reaction kinetics indicate that Cu-SAPO-34 samples formed using SSIE have core-shell structures where Cu is enriched in the shell layers; while Cu is more evenly distributed within the one-pot samples. Reaction kinetics also suggest that at low temperatures, the local environment next to Cu2+ ion centers plays little role on the overall catalytic properties. The authors gratefully acknowledge the US Department of Energy (DOE), Energy Efficiency and Renewable Energy, Vehicle Technologies Office for the support of this work. The research described in this paper was performed at the Environmental

  12. Synthesis and Surface Reactivity of Vinylized Macroporous Silica Monoliths: One-Pot Hybrid versus Postsynthesis Grafting Strategies.

    PubMed

    El-Debs, Racha; Cadoux, Franck; Bois, Laurence; Bonhommé, Anne; Randon, Jérôme; Dugas, Vincent; Demesmay, Claire

    2015-10-27

    Different synthesis routes have been implemented to prepare macroporous monoliths with vinyl pendant groups and micrometric skeletons and through-pore sizes. A standard process combining the synthesis of a widely used (methyltrimethoxysilane/tetramethoxysilane) (MTMS/TMOS) hybrid silica monolith and the postsilanization with vinyltrimethoxysilane (VTMS) was used as reference material (Vgr-MTMS). An alternative "one-pot" procedure was used to obtain vinylized hybrid monoliths. Two VTMS/TMOS hybrid based monoliths were successfully prepared starting from 20% (w) and 80% (w/w) of VTMS, respectively, called 20-VTMS and 80-VTMS. Monoliths were characterized by SEM, nitrogen-adsorption isotherm, and (29)Si MAS NMR spectroscopy. One-pot synthesis allowed to obtain higher vinyl contents (15.9 and 61.5 mol % of Si atoms bonded to vinyl groups respectively for 20-VTMS and 80-VTMS) than for the postgrafted one (7.1%). Accessibility of vinyl groups was determined by the extent of bromination reactions followed by FTIR-ATR spectroscopy. Bromination with reaction yields were higher than 80% for all materials (80%, 85%, and 100% for 80-VTMS, 20-VTMS, and Vgr-MTMS respectively), with no diffusion issues The chemical reactivity of the pendant vinyl groups was investigated through radical-mediated thiol-ene reaction and radical-initiated bisulfite addition. Reaction yields for the two VTMS hybrid monoliths were quite lower (4-6%) than those obtained (about 50%) for the Vgr-MTMS monolith. The difference in reactivity was attributed to the steric hindrance of the vinyl moieties at the surface of hybrid materials. However, the lower reactivity of vinyl groups is compensated by their considerably higher surface density. Thus, hybrid monoliths are advantageous over their grafted counterparts, due to their higher hydrolytic stability and to the greater simplicity of the one-pot process. A chromatographic application exemplifies their interest and performances in separation science. PMID

  13. Synthesis and Surface Reactivity of Vinylized Macroporous Silica Monoliths: One-Pot Hybrid versus Postsynthesis Grafting Strategies.

    PubMed

    El-Debs, Racha; Cadoux, Franck; Bois, Laurence; Bonhommé, Anne; Randon, Jérôme; Dugas, Vincent; Demesmay, Claire

    2015-10-27

    Different synthesis routes have been implemented to prepare macroporous monoliths with vinyl pendant groups and micrometric skeletons and through-pore sizes. A standard process combining the synthesis of a widely used (methyltrimethoxysilane/tetramethoxysilane) (MTMS/TMOS) hybrid silica monolith and the postsilanization with vinyltrimethoxysilane (VTMS) was used as reference material (Vgr-MTMS). An alternative "one-pot" procedure was used to obtain vinylized hybrid monoliths. Two VTMS/TMOS hybrid based monoliths were successfully prepared starting from 20% (w) and 80% (w/w) of VTMS, respectively, called 20-VTMS and 80-VTMS. Monoliths were characterized by SEM, nitrogen-adsorption isotherm, and (29)Si MAS NMR spectroscopy. One-pot synthesis allowed to obtain higher vinyl contents (15.9 and 61.5 mol % of Si atoms bonded to vinyl groups respectively for 20-VTMS and 80-VTMS) than for the postgrafted one (7.1%). Accessibility of vinyl groups was determined by the extent of bromination reactions followed by FTIR-ATR spectroscopy. Bromination with reaction yields were higher than 80% for all materials (80%, 85%, and 100% for 80-VTMS, 20-VTMS, and Vgr-MTMS respectively), with no diffusion issues The chemical reactivity of the pendant vinyl groups was investigated through radical-mediated thiol-ene reaction and radical-initiated bisulfite addition. Reaction yields for the two VTMS hybrid monoliths were quite lower (4-6%) than those obtained (about 50%) for the Vgr-MTMS monolith. The difference in reactivity was attributed to the steric hindrance of the vinyl moieties at the surface of hybrid materials. However, the lower reactivity of vinyl groups is compensated by their considerably higher surface density. Thus, hybrid monoliths are advantageous over their grafted counterparts, due to their higher hydrolytic stability and to the greater simplicity of the one-pot process. A chromatographic application exemplifies their interest and performances in separation science.

  14. One-pot synthesis and cytotoxicity studies of new Mannich base derivatives of polyether antibiotic--lasalocid acid.

    PubMed

    Huczyński, Adam; Rutkowski, Jacek; Borowicz, Izabela; Wietrzyk, Joanna; Maj, Ewa; Brzezinski, Bogumil

    2013-09-15

    Seven Mannich base derivatives of polyether antibiotic Lasalocid acid (2a-2g) were synthesized and screened for their antiproliferative activity against various human cancer cell lines. A novel chemoselective one-pot synthesis of these Mannich bases was developed. Compounds 2a-2c and 2g with sterically smaller dialkylamine substituent, displayed potent antiproliferative activity (IC50: 3.2-7.3 μM), and demonstrated higher than twofold selectivity for specific type of cancer. The nature of Mannich base substituent on C-2 atom at the aromatic ring may be critical in the search for selectivity towards a particular cancer cell. PMID:23932361

  15. New one-pot synthesis of Au and Ag nanoparticles using green rust reactive particle as a micro-reactor.

    PubMed

    Ayadi, Sondra; Perca, Cristian; Legrand, Ludovic

    2013-01-01

    A new, simple, and fast one-pot synthesis of supported Au or Ag nanoparticles is implemented, for which a reactive Fe(II)-bearing green rust inorganic particle is used as an individual micro-reactor acting as both the reducing agent and support for the resulting metal nanoparticles. The mechanism involves both the solid-state oxidation of the green rust support (sulfate or carbonate) and the reduction-precipitation of soluble metal precursor. The resulting nanohybrids have a platy inorganic part supporting about one to ten nanoparticles with sizes in the 20 to 120 nm range. PMID:23433071

  16. New one-pot synthesis of Au and Ag nanoparticles using green rust reactive particle as a micro-reactor

    NASA Astrophysics Data System (ADS)

    Ayadi, Sondra; Perca, Cristian; Legrand, Ludovic

    2013-02-01

    A new, simple, and fast one-pot synthesis of supported Au or Ag nanoparticles is implemented, for which a reactive Fe(II)-bearing green rust inorganic particle is used as an individual micro-reactor acting as both the reducing agent and support for the resulting metal nanoparticles. The mechanism involves both the solid-state oxidation of the green rust support (sulfate or carbonate) and the reduction-precipitation of soluble metal precursor. The resulting nanohybrids have a platy inorganic part supporting about one to ten nanoparticles with sizes in the 20 to 120 nm range.

  17. New one-pot synthesis of Au and Ag nanoparticles using green rust reactive particle as a micro-reactor.

    PubMed

    Ayadi, Sondra; Perca, Cristian; Legrand, Ludovic

    2013-02-22

    A new, simple, and fast one-pot synthesis of supported Au or Ag nanoparticles is implemented, for which a reactive Fe(II)-bearing green rust inorganic particle is used as an individual micro-reactor acting as both the reducing agent and support for the resulting metal nanoparticles. The mechanism involves both the solid-state oxidation of the green rust support (sulfate or carbonate) and the reduction-precipitation of soluble metal precursor. The resulting nanohybrids have a platy inorganic part supporting about one to ten nanoparticles with sizes in the 20 to 120 nm range.

  18. One-pot, three-component approach to the synthesis of 3,4,5-trisubstituted pyrazoles.

    PubMed

    Kamal, Ahmed; Sastry, K N Visweswara; Chandrasekhar, D; Mani, Geeta Sai; Adiyala, Praveen Reddy; Nanubolu, Jagadeesh Babu; Singarapu, Kiran Kumar; Maurya, Ram Awatar

    2015-05-01

    An operationally simple and high yielding protocol for the synthesis of polyfunctional pyrazoles has been developed through one-pot, three-component coupling of aldehydes, 1,3-dicarbonyls, and diazo compounds as well as tosyl hydrazones. The reaction proceeds through a tandem Knoevenagel condensation, 1,3-dipolar cycloaddition, and transition metal-free oxidative aromatization reaction sequence utilizing molecular oxygen as a green oxidant. The scope of the reaction was studied by varying the aldehyde, 1,3-dicarbonyl, and diazo component individually. PMID:25849582

  19. One-pot, three-component approach to the synthesis of 3,4,5-trisubstituted pyrazoles.

    PubMed

    Kamal, Ahmed; Sastry, K N Visweswara; Chandrasekhar, D; Mani, Geeta Sai; Adiyala, Praveen Reddy; Nanubolu, Jagadeesh Babu; Singarapu, Kiran Kumar; Maurya, Ram Awatar

    2015-05-01

    An operationally simple and high yielding protocol for the synthesis of polyfunctional pyrazoles has been developed through one-pot, three-component coupling of aldehydes, 1,3-dicarbonyls, and diazo compounds as well as tosyl hydrazones. The reaction proceeds through a tandem Knoevenagel condensation, 1,3-dipolar cycloaddition, and transition metal-free oxidative aromatization reaction sequence utilizing molecular oxygen as a green oxidant. The scope of the reaction was studied by varying the aldehyde, 1,3-dicarbonyl, and diazo component individually.

  20. New one-pot synthesis of Au and Ag nanoparticles using green rust reactive particle as a micro-reactor

    PubMed Central

    2013-01-01

    A new, simple, and fast one-pot synthesis of supported Au or Ag nanoparticles is implemented, for which a reactive Fe(II)-bearing green rust inorganic particle is used as an individual micro-reactor acting as both the reducing agent and support for the resulting metal nanoparticles. The mechanism involves both the solid-state oxidation of the green rust support (sulfate or carbonate) and the reduction-precipitation of soluble metal precursor. The resulting nanohybrids have a platy inorganic part supporting about one to ten nanoparticles with sizes in the 20 to 120 nm range. PMID:23433071

  1. Facile rhenium-peptide conjugate synthesis using a one-pot derived Re(CO)3 reagent.

    PubMed

    Chanawanno, Kullapa; Kondeti, Vinay; Caporoso, Joel; Paruchuri, Sailaja; Leeper, Thomas C; Herrick, Richard S; Ziegler, Christopher J

    2016-03-21

    We have synthesized two Re(CO)3-modified lysine complexes (1 and 2), where the metal is attached to the amino acid at the Nε position, via a one-pot Schiff base formation reaction. These compounds can be used in the solid phase synthesis of peptides, and to date we have produced four conjugate systems incorporating neurotensin, bombesin, leutenizing hormone releasing hormone, and a nuclear localization sequence. We observed uptake into human umbilical vascular endothelial cells as well as differential uptake depending on peptide sequence identity, as characterized by fluorescence and rhenium elemental analysis. PMID:26863280

  2. One-pot synthesis of stable colloidal solutions of MFe{sub 2}O{sub 4} nanoparticles using oleylamine as solvent and stabilizer

    SciTech Connect

    Pérez-Mirabet, Leonardo; Solano, Eduardo; Martínez-Julián, Fernando; Guzmán, Roger; Arbiol, Jordi; Puig, Teresa; Obradors, Xavier; Pomar, Alberto; Yáñez, Ramón; Ros, Josep; Ricart, Susagna

    2013-03-15

    Highlights: ► One-pot synthesis of ferrite magnetic nanoparticles (<10 nm) in non-polar media. ► Nanoparticles present high monocrystal quality and monodispersion. ► Superparamagnetic behavior at room temperature. ► Nanoparticles transfer to polar media via ligand exchange. - Abstract: An easy, efficient, reproducible and scalable one-pot synthetic methodology to obtain magnetic spinel ferrite nanoparticles has been developed. This approach is based on one-pot thermal decomposition of Fe(acac){sub 3} and M(acac){sub 2} (M = Co, Mn, Cu and Zn) in oleylamine, which also acts as a capping ligand, by producing stable colloidal dispersions of nanoparticles in non-polar solvents. The properties of the nanoparticles have been studied via different techniques, such as transmission electron microscopy, which shows that nanoparticles are monocrystallines and a narrow dispersion in size; magnetic analyses have demonstrated that the resulting ferrite nanoparticles show high saturation values and superparamagnetic behavior at room temperature; X-ray diffraction has also been performed, and it confirms that the synthesized nanoparticles have a spinel structure. Complementarily, ligand exchange has been also carried out in order to produce dispersions of the synthesized nanoparticles in polar media.

  3. A mild, three-component one-pot synthesis of 2,4,5-trisubstituted imidazoles using Mo(IV) salen complex in homogeneous catalytic system and Mo(IV) salen complex nanoparticles onto silica as a highly active, efficient, and reusable heterogeneous nanocatalyst.

    PubMed

    Sharghi, Hashem; Aberi, Mahdi; Doroodmand, Mohammad Mahdi

    2015-02-01

    Mo(IV) salen complex (2.5 mol%) was found to be a highly efficient catalyst for the one-pot synthesis of 2,4,5-triarylimidazoles via a three-component reaction using benzil or benzoin, aryl aldehydes, and ammonium acetate as a nitrogen source under mild conditions. In order to recover and the reuse of the catalyst, a new Mo(IV) salen-silica nanoparticle as heterogeneous catalyst was prepared by simple and successful immobilization of the catalyst onto silica (3-aminopropyl functionalized silica gel). This procedure can be applied to large-scale conditions with high efficiency. Experimental evidence showed that the catalyst is stable and can be easily recovered and reused for at least five times without significant loss of activity. The nanocatalyst was characterized using FT-IR spectroscopy, scanning electron microscopy, atomic force microscopy, powder X-ray diffraction , transmission electron microscopy, thermogravimetric instrument for analysis of nitrogen adsorption, and inductively coupled plasma spectrometer. PMID:25515148

  4. One-pot synthesis of active copper-containing carbon dots with laccase-like activities

    NASA Astrophysics Data System (ADS)

    Ren, Xiangling; Liu, Jing; Ren, Jun; Tang, Fangqiong; Meng, Xianwei

    2015-11-01

    Herein, an effective strategy for designing a new type of nanozyme, blue fluorescent laccase mimics, is reported. Active copper-containing carbon dots (Cu-CDs) were synthesized through a simple, nontoxic and one-pot hydrothermal method, which showed favorable photoluminescence properties and good photostability under high-salt conditions or in a broad pH range (3.0-13.5). The Cu-CDs possessed intrinsic laccase-like activities and could catalyze the oxidation of the laccase substrate p-phenylenediamine (PPD) to produce a typical color change from colorless to brown. Poly(methacrylic acid sodium salt) (PMAA) not only was used as the carbon source and reducing agent, but also provided carboxyl groups to assist flocculation between Cu-CDs and polyacrylamide, which facilitated the removal of PPD. Importantly, the intrinsic fluorescence of the as-prepared Cu-CDs could indicate the presence of hydroquinone, one of the substrates of laccases, based on laccase mimics and fluorescence quenching.Herein, an effective strategy for designing a new type of nanozyme, blue fluorescent laccase mimics, is reported. Active copper-containing carbon dots (Cu-CDs) were synthesized through a simple, nontoxic and one-pot hydrothermal method, which showed favorable photoluminescence properties and good photostability under high-salt conditions or in a broad pH range (3.0-13.5). The Cu-CDs possessed intrinsic laccase-like activities and could catalyze the oxidation of the laccase substrate p-phenylenediamine (PPD) to produce a typical color change from colorless to brown. Poly(methacrylic acid sodium salt) (PMAA) not only was used as the carbon source and reducing agent, but also provided carboxyl groups to assist flocculation between Cu-CDs and polyacrylamide, which facilitated the removal of PPD. Importantly, the intrinsic fluorescence of the as-prepared Cu-CDs could indicate the presence of hydroquinone, one of the substrates of laccases, based on laccase mimics and fluorescence quenching

  5. One-pot synthesis of ferrocenyl ketones containing biaryls and 6-aryl-2-ferrocenylquinolines via Ir/Pd-cocatalyzed α-alkylation/Suzuki reaction.

    PubMed

    Xu, Chen; Hao, Xin-Qi; Xiao, Zhi-Qiang; Wang, Zhi-Qiang; Yuan, Xiao-Er; Fu, Wei-Jun; Ji, Bao-Ming; Song, Mao-Ping

    2013-09-01

    An efficient PPh3-cyclometalated iridium(III) benzo[h]quinoline hydride 1/Pd(OAc)2-cocatalyzed three-component α-alkylation/Suzuki reaction has been developed. The three-component reaction of 4-bromobenzyl alcohol, acetylferrocene, and arylboronic acids gives ferrocenyl ketones containing biaryls in moderate to good yields. This method was successfully applied to a one-pot synthesis of 6-aryl-2-ferrocenyl quinolines, using (2-amino-5-bromophenyl)methanol instead of 4-bromobenzyl alcohol. PMID:23924342

  6. One-pot synthesis of active copper-containing carbon dots with laccase-like activities.

    PubMed

    Ren, Xiangling; Liu, Jing; Ren, Jun; Tang, Fangqiong; Meng, Xianwei

    2015-12-14

    Herein, an effective strategy for designing a new type of nanozyme, blue fluorescent laccase mimics, is reported. Active copper-containing carbon dots (Cu-CDs) were synthesized through a simple, nontoxic and one-pot hydrothermal method, which showed favorable photoluminescence properties and good photostability under high-salt conditions or in a broad pH range (3.0-13.5). The Cu-CDs possessed intrinsic laccase-like activities and could catalyze the oxidation of the laccase substrate p-phenylenediamine (PPD) to produce a typical color change from colorless to brown. Poly(methacrylic acid sodium salt) (PMAA) not only was used as the carbon source and reducing agent, but also provided carboxyl groups to assist flocculation between Cu-CDs and polyacrylamide, which facilitated the removal of PPD. Importantly, the intrinsic fluorescence of the as-prepared Cu-CDs could indicate the presence of hydroquinone, one of the substrates of laccases, based on laccase mimics and fluorescence quenching. PMID:26548709

  7. One-pot synthesis and antimicrobial evaluation of novel 3-cyanopyridine derivatives of (-)-β-pinene.

    PubMed

    Liao, Shengliang; Shang, Shibin; Shen, Minggui; Rao, Xiaoping; Si, Hongyan; Song, Jie; Song, Zhanqian

    2016-03-15

    A series of novel 3-cyanopyridine derivatives of (-)-β-pinene were designed and synthesized by one-pot four-component domino reactions. The targeted compounds were evaluated for their antimicrobial activity against four bacteria (Klebsiella pneumoniae, Enterobacter aerogenes, Staphylococcus aureus, Staphylococcus epidermidis) and a fungus (Candida albicans). The results showed that most of the minimal inhibitory concentrations (MICs) of these 3-cyanopyridine derivatives against the tested strains was in the range of 15.6-125 mg/L. Among these 3-cyanopyridine derivatives, the MICs of compound 5h against S. epidermidis and C. albicans were 15.6 mg/L, which revealed that compound 5h featured double fluoro substituents at meta- and para-position was the most active compound. In addition, the preliminary structure-activity relationship analysis indicated that the change of substituents on the pyridine ring and benzene ring of 3-cyanopyridine derivatives was an important factor for inducing antimicrobial activity. This research would promote the development of heterocyclic derivatives of β-pinene with antimicrobial activity. PMID:26898336

  8. One-pot synthesis of monodisperse 5 nm Pd-Ni nanoalloys for electrocatalytic ethanol oxidation.

    PubMed

    Lee, Kyungwon; Kang, Shin Wook; Lee, Su-Un; Park, Kyu-Hwan; Lee, Young Wook; Han, Sang Woo

    2012-08-01

    Highly monodisperse 5 nm Pd-Ni alloy nanoparticles (NPs) were prepared by the reduction of Pd(acac)(2)/Ni(acac)(2) mixtures with tert-butylamine-borane complex (TBAB) in the presence of oleic acid (OA) and oleylamine (OAm). Employing TBAB as an effective reductant and OA/OAm combination as an effective stabilizing agent is crucial to the formation of monodisperse Pd-Ni NPs. Experimental results collectively verify that the Pd-Ni alloy NPs form through the sequential nucleation-interdiffusion process and the simultaneous reduction of both metal precursors by the one-pot protocol is the key to the formation of homogeneous NPs. The Pd-Ni NPs were well-dispersed on carbon supports and chemically dealloyed after acetic acid washing through the selective dissolution of the less noble Ni component. The Pd-Ni NP catalysts exhibited much higher electrocatalytic activity and stability for ethanol oxidation than those of a commercial Pd/C catalyst.

  9. One-pot synthesis and antimicrobial evaluation of novel 3-cyanopyridine derivatives of (-)-β-pinene.

    PubMed

    Liao, Shengliang; Shang, Shibin; Shen, Minggui; Rao, Xiaoping; Si, Hongyan; Song, Jie; Song, Zhanqian

    2016-03-15

    A series of novel 3-cyanopyridine derivatives of (-)-β-pinene were designed and synthesized by one-pot four-component domino reactions. The targeted compounds were evaluated for their antimicrobial activity against four bacteria (Klebsiella pneumoniae, Enterobacter aerogenes, Staphylococcus aureus, Staphylococcus epidermidis) and a fungus (Candida albicans). The results showed that most of the minimal inhibitory concentrations (MICs) of these 3-cyanopyridine derivatives against the tested strains was in the range of 15.6-125 mg/L. Among these 3-cyanopyridine derivatives, the MICs of compound 5h against S. epidermidis and C. albicans were 15.6 mg/L, which revealed that compound 5h featured double fluoro substituents at meta- and para-position was the most active compound. In addition, the preliminary structure-activity relationship analysis indicated that the change of substituents on the pyridine ring and benzene ring of 3-cyanopyridine derivatives was an important factor for inducing antimicrobial activity. This research would promote the development of heterocyclic derivatives of β-pinene with antimicrobial activity.

  10. One-pot synthesis of active copper-containing carbon dots with laccase-like activities.

    PubMed

    Ren, Xiangling; Liu, Jing; Ren, Jun; Tang, Fangqiong; Meng, Xianwei

    2015-12-14

    Herein, an effective strategy for designing a new type of nanozyme, blue fluorescent laccase mimics, is reported. Active copper-containing carbon dots (Cu-CDs) were synthesized through a simple, nontoxic and one-pot hydrothermal method, which showed favorable photoluminescence properties and good photostability under high-salt conditions or in a broad pH range (3.0-13.5). The Cu-CDs possessed intrinsic laccase-like activities and could catalyze the oxidation of the laccase substrate p-phenylenediamine (PPD) to produce a typical color change from colorless to brown. Poly(methacrylic acid sodium salt) (PMAA) not only was used as the carbon source and reducing agent, but also provided carboxyl groups to assist flocculation between Cu-CDs and polyacrylamide, which facilitated the removal of PPD. Importantly, the intrinsic fluorescence of the as-prepared Cu-CDs could indicate the presence of hydroquinone, one of the substrates of laccases, based on laccase mimics and fluorescence quenching.

  11. Sulfamic acid promoted one-pot three-component synthesis and cytotoxic evaluation of spirooxindoles.

    PubMed

    Kamal, Ahmed; Babu, Korrapati Suresh; Vishnu Vardhan, M V P S; Hussaini, S M Ali; Mahesh, Rasala; Shaik, Siddiq Pasha; Alarifi, Abdullah

    2015-01-01

    A simple, mild and efficient method for the synthesis of pyrazolopyridine based spirooxindoles by the three-component reaction has been developed using sulfamic acid (H2NSO3H) as a green catalyst. The method involves use of water as a solvent which makes it eco-friendly. The catalyst used is readily available and is prominent for short reaction time, operational simplicity and high yields. After completion of the reaction the catalyst could be recovered and reused for up to four cycles without loss in catalytic activity. Employing this method a library of 34 compounds has been synthesized and investigated for their cytotoxicity against a panel of three human cancer cell lines. Some of the compounds like 4o and 4p exhibited remarkable cytotoxicities with IC50 values of 0.35μM and 1.92μM against MDA-MB-231 cell line. PMID:25870131

  12. The first one-pot synthesis of metal-organic frameworks functionalised with two transition-metal complexes.

    PubMed

    Platero-Prats, Ana E; Bermejo Gómez, Antonio; Samain, Louise; Zou, Xiaodong; Martín-Matute, Belén

    2015-01-01

    The synthesis of a metal-organic framework (UiO-67) functionalised simultaneously with two different transition metal complexes (Ir and Pd or Rh) through a one-pot procedure is reported for the first time. This has been achieved by an iterative modification of the synthesis parameters combined with characterisation of the resulting materials using different techniques, including X-ray absorption spectroscopy (XAS). The method also allows the first synthesis of UiO-67 with a very wide range of loadings (from 4 to 43 mol %) of an iridium complex ([IrCp*(bpydc)(Cl)Cl](2-) ; bpydc=2,2'-bipyridine-5,5'-dicarboxylate, Cp*=pentamethylcyclopentadienyl) through a pre-functionalisation methodology.

  13. Baylis-Hillman acetates in organic synthesis: convenient one-pot synthesis of α-carboline framework--a concise synthesis of neocryptolepine.

    PubMed

    Basavaiah, Deevi; Mallikarjuna Reddy, Daggula

    2012-11-28

    A convenient, facile, and one-pot methodology for the synthesis of α-carbolines from Baylis-Hillman (BH) acetates, involving three steps (reactions), (1) mono alkylation of 2-nitroarylacetonitriles with BH-acetates, (2) reduction of nitro group into amino group using Fe/AcOH and (3) formation of two (five and six membered) rings, is presented. This methodology is successfully applied to the synthesis of bioactive alkaloid neocryptolepine.

  14. One-pot synthesis of two-sized clusters for ratiometric sensing of Hg2+.

    PubMed

    Chen, Tzu-Heng; Lu, Chi-Yu; Tseng, Wei-Lung

    2013-12-15

    This paper presents a discussion of a one-pot approach for preparing lyszoyme type VI (Lys VI) stabilized clusters, including small (Au7Ag and Au8) and large (Au24Ag) clusters, for ratiometric fluorescence sensing of Hg(2+). Our previous study (Chen and Tseng, Small 8 (2012) 1912) showed the formation of intermediate Au8 clusters in the conversion of Au(+)-Lys VI protein complexes to Au25 clusters. The presence of Ag(+) in the precursor solution slowed this conversion, thereby forming two-sized clusters. With an increase in Ag(+) content, a systematic blue shift in the first exciton absorption and fluorescence peaks indicated the formation of Au-Ag bimetallic clusters. The prepared Ag(+)/Au(3+) molar ratio of 2:8 resulted in the formation of two-sized clusters, with dual emission bands centered at 471 and 613 nm. After these clusters are separated by a membrane filter, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry was used to determine the composition of Au24Ag clusters. By monitoring the intensity ratio of the two emission wavelengths, the solution consisting of Hg(2+)-insensitive small clusters (Au7Ag and Au8) and Hg(2+)-sensitive Au24Ag clusters exhibited a ratiometric fluorescence response toward Hg(2+), and provided a built-in correction for photobleaching; the limit of detection at a signal-to-noise ratio of three for Hg(2+) was estimated to be 1 nM. This probe was successfully applied to ratiometric fluorescence sensing of Hg(2+) in tap water. PMID:24209338

  15. One-pot multiple reactions: asymmetric synthesis of 2,6-cis-disubstituted piperidine alkaloids from chiral aziridine.

    PubMed

    Yadav, Nagendra Nath; Choi, Jihye; Ha, Hyun-Joon

    2016-07-01

    A divergent, new, and highly stereoselective synthesis of cis-2,6-disubstituted piperidine natural products including isosolenopsins, deoxocassine, and spectaline was achieved from chiral aziridine decorated with appropriate alkyl chains for isosolenopsins or alkynyl groups for deoxocassine and spectaline at C2. The characteristic feature of this synthesis is one-pot sequential reactions under atmospheric hydrogen including the reduction of alkyne (for deoxocassine and spectaline), reductive ring-opening of aziridine, debenzylation, and intramolecular reductive amination in high yields. The prerequisite aziridines were elaborated from commercially available (2S)-hydroxymethylaziridine through oxidation, Wittig olefination, and the Grignard reaction for isosolenopsins or substrate-controlled lithium alkynylate addition for deoxocassine and spectaline. PMID:27189444

  16. Multicomponent One-pot Reactions Towards the Synthesis of Stereoisomers of Dipicolylamine Complexes.

    PubMed

    Raje, Sakthi; Gurusamy, Sureshbabu; Koner, Abhishek; Mehrotra, Sonam; Jennifer, Samson Jegan; Vasudev, Prema G; Butcher, Ray J; Angamuthu, Raja

    2016-01-01

    Reported are multi-component one-pot syntheses of chiral complexes [M(L(R) OR')Cl2 ] or [M(L(R) SR')Cl2 ] from the mixture of an N-substituted ethylenediamine, pyridine-2-carboxaldehyde, a primary alcohol or thiol and MCl2 utilizing in-situ formed cyclized Schiff bases where a C-O bond, two stereocenters, and three C-N bonds are formed (M=Zn, Cu, Ni, Cd; R=Et, Ph; R'=Me, Et, nPr, nBu). Tridentate ligands L(R) OR' and L(R) SR' comprise two chiral centers and a hemiaminal ether or hemiaminal thioether moiety on the dipicolylamine skeleton. Syn-[Zn(L(Ph) OMe)Cl2 ] precipitates out readily from the reaction mixture as a major product whereas anti-[Zn(L(Ph) OMe)Cl2 ] stays in solution as minor product. Both syn-[Zn(L(Ph) OMe)Cl2 ] and anti-[Zn(L(Ph) OMe)Cl2 ] were characterized using NMR spectroscopy and mass spectrometry. Solid-state structures revealed that syn-[Zn(L(Ph) OMe)Cl2 ] adopted a square pyramidal geometry while anti-[Zn(L(Ph) OMe)Cl2 ] possesses a trigonal bipyramidal geometry around the Zn centers. The scope of this method was shown to be wide by varying the components of the dynamic coordination assembly, and the structures of the complexes isolated were confirmed by NMR spectroscopy, mass spectrometry, and X-ray crystallography. Syn complexes were isolated as major products with Zn(II) and Cu(II) , and anti complexes were found to be major products with Ni(II) and Cd(II) . Hemiaminals and hemiaminal ethers are known to be unstable and are seldom observed as part of cyclic organic compounds or as coordinated ligands assembled around metals. It is now shown, with the support of experimental results, that linear hemiaminal ethers or thioethers can be assembled without the assistance of Lewis acidic metals in the multi-component assembly, and a possible pathway of the formation of hemiaminal ethers has been proposed.

  17. One-Pot Synthesis of Substituted Benzo[b]furans and Indoles from Dichlorophenols/Dichloroanilines Using a Palladium-Dihydroxyterphenylphosphine Catalyst.

    PubMed

    Yamaguchi, Miyuki; Akiyama, Tomoyo; Sasou, Hirohisa; Katsumata, Haruka; Manabe, Kei

    2016-07-01

    Disubstituted benzo[b]furans were synthesized by ortho-selective Sonogashira coupling of dichlorophenols and terminal alkynes, followed by cyclization and Suzuki-Miyaura coupling in one pot, using a palladium-dihydroxyterphenylphosphine (Cy-DHTP) catalyst. The use of substoichiometric amounts of tetrabutylammonium chloride was effective in accelerating the Suzuki-Miyaura coupling. This protocol was also successfully applied to the one-pot synthesis of disubstituted indoles from dichloroaniline derivatives.

  18. Synthesis of dibenzoxepine lactams via a Cu-catalyzed one-pot etherification/aldol condensation cascade reaction: application toward the total synthesis of aristoyagonine.

    PubMed

    Lim, Hye Sun; Choi, Young Lok; Heo, Jung-Nyoung

    2013-09-20

    A general synthesis of dibenzoxepine lactams has been developed using a one-pot Cu-catalyzed etherification/aldol condensation cascade reaction. The reaction of 4-hydroxyisoindolin-1-one with a wide range of 2-bromobenzaldehydes in the presence of a copper catalyst provided various aristoyagonine derivatives in good yields. PMID:24000941

  19. A one-pot, three-step process for the diastereoselective synthesis of aminobicyclo[4.3.0]nonanes using consecutive palladium(II)- and ruthenium(II)-catalysis.

    PubMed

    Mostafa, Mohamed A B; Grafton, Mark W; Wilson, Claire; Sutherland, Andrew

    2016-03-28

    A diastereoselective synthesis of highly substituted aminobicyclo[4.3.0]nonanes has been attained using a one-pot multi-bond forming process. A four-step synthetic route was developed for the efficient synthesis of a series of C-7 substituted hept-2-en-6-yn-1-ols. These compounds were then investigated as substrates for a one-pot, three-step tandem process involving a palladium(ii)-catalysed Overman rearrangement, a ruthenium(ii)-catalysed ring closing enyne metathesis reaction followed by a hydrogen bond directed Diels-Alder reaction. The optimisation of the one-pot process has allowed the rapid preparation of a library of aminobicyclo[4.3.0]nonanes with significant molecular complexity and up to four stereogenic centres.

  20. A one-pot, three-step process for the diastereoselective synthesis of aminobicyclo[4.3.0]nonanes using consecutive palladium(II)- and ruthenium(II)-catalysis.

    PubMed

    Mostafa, Mohamed A B; Grafton, Mark W; Wilson, Claire; Sutherland, Andrew

    2016-03-28

    A diastereoselective synthesis of highly substituted aminobicyclo[4.3.0]nonanes has been attained using a one-pot multi-bond forming process. A four-step synthetic route was developed for the efficient synthesis of a series of C-7 substituted hept-2-en-6-yn-1-ols. These compounds were then investigated as substrates for a one-pot, three-step tandem process involving a palladium(ii)-catalysed Overman rearrangement, a ruthenium(ii)-catalysed ring closing enyne metathesis reaction followed by a hydrogen bond directed Diels-Alder reaction. The optimisation of the one-pot process has allowed the rapid preparation of a library of aminobicyclo[4.3.0]nonanes with significant molecular complexity and up to four stereogenic centres. PMID:26932788

  1. One-Pot Synthesis of Aza-Diketopiperazines Enabled by Controlled Reactivity of N-Isocyanate Precursors.

    PubMed

    Ivanovich, Ryan A; Vincent-Rocan, Jean-François; Elkaeed, Eslam B; Beauchemin, André M

    2015-10-01

    A one-pot sequence for the synthesis of aza-diketopiperazines is reported, involving carbazate acylation with chloroacetyl chloride, SN2 with a primary amine, N-isocyanate formation, and cyclization. Nitrogen-substituted isocyanates (N-isocyanates) are a rare class of amphoteric isocyanate with high, but severely underdeveloped synthetic potential. This approach highlights that βN-acyl carbazates can act as blocked (masked) N-isocyanates, thus allowing a challenging intermolecular SN2 reaction of a primary amine to proceed while the N-isocyanate is "protected", and then cyclization once it is unmasked. Control experiments show that the alternate pathway--N-isocyanate substitution and then cyclization by an intramolecular SN2 reaction--is not operating.

  2. One-pot aqueous synthesis of gadolinium doped CdTe quantum dots with dual imaging modalities.

    PubMed

    Jiang, Chunli; Shen, Zhitao; Luo, Chunhua; Lin, Hechun; Huang, Rong; Wang, Yiting; Peng, Hui

    2016-08-01

    A facile one-pot strategy has been developed for the aqueous synthesis of Gd doped CdTe (Gd:CdTe) QDs as fluorescence and magnetic resonance imaging dual-modal agent. The prepared Gd:CdTe QDs showed narrow size distribution and the average size was less than 5nm. The amount of Gd(3+) dopant in Gd:CdTe QDs significantly affected the optical properties of obtained QDs. The highest PL QY for the prepared Gd:CdTe QDs was up to 42.5%. The QDs showed the weak toxicity and significant enhancement in MRI signal. The specific relaxivity value (r1) was determined to be 4.22mM(-1)s(-1). These properties make the prepared Gd:CdTe QDs be an effective dual-modal imaging agent and have great potential applications in biomedical field.

  3. Amide-controlled, one-pot synthesis of tri-substituted purines generates structural diversity and analogues with trypanocidal activity.

    PubMed

    Pineda de las Infantas y Villatoro, Maria J; Unciti-Broceta, Juan D; Contreras-Montoya, Rafael; Garcia-Salcedo, Jose A; Gallo Mezo, Miguel A; Unciti-Broceta, Asier; Diaz-Mochon, Juan J

    2015-01-01

    A novel one-pot synthesis of tri-substituted purines and the discovery of purine analogues with trypanocidal activity are reported. The reaction is initiated by a metal-free oxidative coupling of primary alkoxides and diaminopyrimidines with Schiff base formation and subsequent annulation in the presence of large N,N-dimethylamides (e.g. N,N-dimethylpropanamide or larger). This synthetic route is in competition with a reaction previously-reported by our group, allowing the generation of a combinatorial library of tri-substituted purines by the simple modification of the amide and the alkoxide employed. Among the variety of structures generated, two purine analogues displayed trypanocidal activity against the protozoan parasite Trypanosoma brucei with IC50 < 5 μM, being each of those compounds obtained through each of the synthetic pathways.

  4. One-pot synthesis of MWW zeolite nanosheets using a rationally designed organic structure-directing agent

    PubMed Central

    Luo, Helen Y.; Michaelis, Vladimir K.; Hodges, Sydney; Griffin, Robert G.

    2015-01-01

    A new material MIT-1 comprised of delaminated MWW zeolite nanosheets is synthesized in one-pot using a rationally designed organic structure-directing agent (OSDA). The OSDA is comprised of a hydrophilic head segment that resembles the OSDA used to synthesize the zeolite precursor MCM22(P), a hydrophobic tail segment that resembles the swelling agent used to swell MCM22(P), and a di-quaternary ammonium linker that connects both segments. MIT-1 features high crystallinity and surface areas exceeding 500 m2g−1, and can be synthesized over a wide synthesis window that includes Si/Al ratios ranging from 13 to 67. Characterization data reveal high mesoporosity and acid strength with no detectable amorphous silica phases. Compared to MCM-22 and MCM-56, MIT-1 shows a three-fold increase in catalytic activity for the Friedel-Crafts alkylation of benzene with benzyl alcohol. PMID:26478803

  5. One-pot aqueous synthesis of gadolinium doped CdTe quantum dots with dual imaging modalities.

    PubMed

    Jiang, Chunli; Shen, Zhitao; Luo, Chunhua; Lin, Hechun; Huang, Rong; Wang, Yiting; Peng, Hui

    2016-08-01

    A facile one-pot strategy has been developed for the aqueous synthesis of Gd doped CdTe (Gd:CdTe) QDs as fluorescence and magnetic resonance imaging dual-modal agent. The prepared Gd:CdTe QDs showed narrow size distribution and the average size was less than 5nm. The amount of Gd(3+) dopant in Gd:CdTe QDs significantly affected the optical properties of obtained QDs. The highest PL QY for the prepared Gd:CdTe QDs was up to 42.5%. The QDs showed the weak toxicity and significant enhancement in MRI signal. The specific relaxivity value (r1) was determined to be 4.22mM(-1)s(-1). These properties make the prepared Gd:CdTe QDs be an effective dual-modal imaging agent and have great potential applications in biomedical field. PMID:27216651

  6. One-pot synthesis of an Fe(II) bis-terpyridine complex with allosterically regulated electronic properties.

    PubMed

    Machan, Charles W; Adelhardt, Mario; Sarjeant, Amy A; Stern, Charlotte L; Sutter, Jörg; Meyer, Karsten; Mirkin, Chad A

    2012-10-17

    Herein we report the one-pot synthesis of Fe(II) bis-terpyridine complexes with two peripheral square-planar Pt(II) bis-phosphinoalkylthioether moieties. These novel structures, which exhibit allosterically controllable electronic properties, are made by taking advantage of two orthogonal and high-yielding reactions. The prototypical complex can be structurally regulated through the reversible abstraction and introduction of chloride ions to the Pt(II) centers. This moves the Fe(II) center and two Pt(II) metal centers into and out of communication with each other, causing changes in the electronic structure of the complex and its corresponding optical and redox properties. The start and end points of the allosterically regulated system have been characterized by single-crystal X-ray diffraction and NMR, UV-vis, and (57)Fe Mößbauer spectroscopy.

  7. One-pot synthesis of biocompatible superparamagnetic iron oxide nanoparticles/hydrogel based on salep: characterization and drug delivery.

    PubMed

    Bardajee, Ghasem Rezanejade; Hooshyar, Zari

    2014-01-30

    This work describes synthesis of biocompatible magnetic iron oxide nanoparticles/hydrogel based on salep (MION-salep hydrogel) by a facile one-pot strategy. The prepared sample was characterized by techniques like scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDAX), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analysis (TGA), and vibrating sample magnetometer (VSM). The obtained MION had an 8 nm diameter with a narrow size distribution and was superparamagnetic with large saturation magnetization at room temperature. The most attractive feature of the obtained sample was its swelling properties under external magnetic field (EMF), different temperatures, and pHs. Moreover, MION-salep hydrogel showed ability to deferasirox release at pH=7 with non-Fickian diffusion mechanism. An in vitro cytotoxicity study implied that the as-synthesized sample is nontoxic.

  8. Solventless and One-Pot Synthesis of Cu(II) Phthalocyanine Complex: A Green Chemistry Experiment

    ERIC Educational Resources Information Center

    Sharma, R. K.; Sharma, Chetna; Sidhwani, Indu Tucker

    2011-01-01

    With the growing awareness of green chemistry, it is increasingly important for students to understand this concept in the context of laboratory experiments. Although microwave-assisted organic synthesis has become a common and invaluable technique in recent years, there have been few procedures published for microwave-assisted inorganic synthesis…

  9. Simplified one-pot synthesis of [.sup.18F]SFB for radiolabeling

    SciTech Connect

    Olma, Sebastian; Shen, Clifton Kwang-Fu

    2015-08-04

    A non-aqueous single pot synthesis of [.sup.18F]SFB is set forth. The [.sup.18F]SFB produced with this method is then used, for example, to label a peptide or an engineered antibody fragment (diabody) targeting human epidermal growth factor receptor 2 (HER2) as representative examples of labeled compounds for use as an injectable composition to locate abnormal tissue, specifically tumors within an animal or human using a PET scan.

  10. Simplified one-pot synthesis of [.sup.18F]SFB for radiolabeling

    DOEpatents

    Olma, Sebastian; Shen, Clifton Kwang-Fu

    2013-07-16

    A non-aqueous single pot synthesis of [.sup.18F]SFB is set forth. The [.sup.18F]SFB produced with this method is then used, for example, to label a peptide or an engineered antibody fragment (diabody) targeting human epidermal growth factor receptor 2 (HER2) as representative examples of labeled compounds for use as an injectable composition to locate abnormal tissue, specifically tumors within an animal or human using a PET scan.

  11. Novel one-pot synthesis of magnetite latex nanoparticles by ultrasound irradiation.

    PubMed

    Teo, Boon M; Chen, Fei; Hatton, T Alan; Grieser, Franz; Ashokkumar, Muthupandian

    2009-03-01

    A simple and efficacious procedure for the synthesis of magnetite nanoparticles has been achieved via a sonochemical miniemulsion polymerization process. The sonochemically synthesized magnetite encapsulated polymer latex particles exhibit excellent colloidal stability and strong magnetic properties, and are of a size that makes them technologically relevant. This novel method may be readily extended to the preparation of multiple combinations of different polymers and encapsulated materials.

  12. Facile one-pot synthesis of polytypic (wurtzite-chalcopyrite) CuGaS2

    NASA Astrophysics Data System (ADS)

    Vahidshad, Yaser; Mirkazemi, Seyed Mohammad; Tahir, Muhammad Nawaz; Zad, Azam Iraji; Ghasemzadeh, Reza; Tremel, Wolfgang

    2016-03-01

    In this investigation, monodisperse CuGaS2 nanoparticles intended for use as visible-light-absorbing materials were synthesized using a facile one-step heating method that involved dissolving the precursors copper chloride, gallium acetylacetonate, and thiourea in a solvent consisting of either oleylamine alone or a combination of oleylamine, oleic acid, and 1-octadecene. The shapes of the resulting nanoparticles were either elongated, polygonal, or a mixture of both, depending on whether the crystal structure of the nanoparticles was predominantly wurtzite, predominantly chalcopyrite, or a more balanced mixture of both wurtzite and chalcopyrite (i.e., the nanoparticles were polytypic: both wurtzite and chalcopyrite phases were present). The crystal structure of the synthesized nanoparticles was found to be influenced by the temperature and the solvent applied during synthesis. X-ray diffraction data for the nanoparticles indicated that applying a temperature of 270 °C or using oleylamine, oleic acid solvent, and 1-octadecene during synthesis tended to yield a chalcopyrite phase, whereas applying a somewhat lower temperature (210 °C) or using oleylamine alone during synthesis tended to result in a wurtzite phase. The chemical states of the compounds obtained at different temperatures and using various solvents, as well as their crystal structures, morphologies, and optical properties were characterized via X-ray photoelectron spectroscopy, X-ray diffraction, transmission electron microscopy, ultraviolet-visible spectroscopy, and photoluminescence.

  13. One-pot SSA-catalyzed β-elimination: An efficient and inexpensive protocol for easy access to the glycal of sialic acid

    PubMed Central

    Paragas, Erickson M.; Monreal, I. Abrrey; Vasil, Chris M.; Saludes, Jonel P.

    2014-01-01

    Neu5Ac2en1Me per-OAc, the fully protected glycal of sialic acid, is a key intermediate in the discovery of therapeutics and diagnostics, including anti-influenza drugs and proteolysis resistant peptidomimetic foldamers. The synthesis of this sialic acid derivative, however, still relies on standard sugar chemistry that utilizes multi-step methodologies. Herein we report a facile and highly efficient microwave-assisted preparation of Neu5Ac1Me using silica sulfuric acid (SSA) as solid-supported acid catalyst that is one- to two-orders of magnitude faster than standard procedures. We also describe the microwave-assisted and SSA-catalyzed one-pot, rapid, solvent free reaction that combines both peracetylation and β-elimination reactions in one step to generate the glycal from Neu5Ac1Me. We coined the term One-pot SSA-catalyzed Technology for β-Elimination Protocol (OneSTEP) to describe this least laborious, most efficient, and practical preparation to date of Neu5Ac2en1Me per-OAc in terms of yield, time, reagent cost, and waste generation. PMID:25497336

  14. Facile one-pot synthesis of gold and silver nanocatalysts using edible coconut oil

    NASA Astrophysics Data System (ADS)

    Meena Kumari, M.; Philip, Daizy

    2013-07-01

    The use of edible oil for the synthesis of metal nanoparticles by wet chemical method is reported for the first time. The paper presents an environmentally benign bottom up approach for the synthesis of gold and silver nanoparticles using edible coconut oil at 373 K. The formation of silver nanoparticles is signaled by the brownish yellow color and that of gold nanoparticles by the purple color. Fine control over the nanoparticle size and shape from triangular to nearly spherical is achieved by varying the quantity of coconut oil. The nanoparticles have been characterized by UV-Visible, Transmission Electron Microscopy and X-ray Diffraction. The chemical interaction of capping agents with metal nanoparticles is manifested using Fourier Transform Infrared Spectroscopy. The stable and crystalline nanoparticles obtained using this simple method show remarkable size-dependent catalytic activity in the reduction of the cationic dye methylene blue (MB) to leuco methylene blue (LMB). The first order rate constants calculated uphold the size dependent catalytic activity of the synthesized nanoparticles.

  15. Facile one-pot synthesis of gold and silver nanocatalysts using edible coconut oil.

    PubMed

    Meena Kumari, M; Philip, Daizy

    2013-07-01

    The use of edible oil for the synthesis of metal nanoparticles by wet chemical method is reported for the first time. The paper presents an environmentally benign bottom up approach for the synthesis of gold and silver nanoparticles using edible coconut oil at 373 K. The formation of silver nanoparticles is signaled by the brownish yellow color and that of gold nanoparticles by the purple color. Fine control over the nanoparticle size and shape from triangular to nearly spherical is achieved by varying the quantity of coconut oil. The nanoparticles have been characterized by UV-Visible, Transmission Electron Microscopy and X-ray Diffraction. The chemical interaction of capping agents with metal nanoparticles is manifested using Fourier Transform Infrared Spectroscopy. The stable and crystalline nanoparticles obtained using this simple method show remarkable size-dependent catalytic activity in the reduction of the cationic dye methylene blue (MB) to leuco methylene blue (LMB). The first order rate constants calculated uphold the size dependent catalytic activity of the synthesized nanoparticles.

  16. One-pot synthesis of triangular gold nanoplates allowing broad and fine tuning of edge length

    NASA Astrophysics Data System (ADS)

    Miranda, Adelaide; Malheiro, Eliana; Skiba, Elżbieta; Quaresma, Pedro; Carvalho, Patrícia A.; Eaton, Peter; de Castro, Baltazar; Shelnutt, John A.; Pereira, Eulália

    2010-10-01

    A photocatalytic approach was used to synthesize triangular nanoplates in aqueous solution. The synthesis is based on the reduction of a gold salt using a tin(iv) porphyrin as photocatalyst, cetyltrimethylammonium bromide (CTAB) as a stabilizing agent, and triethanolamine (TEA) as the final electron donor. The average edge length of the triangular nanoplates can be easily changed in the range 45-250 nm by varying the concentration of photocatalyst, and fine-tuning of the average edge length is achieved by varying the concentration of CTAB. Study of the mechanism of formation of the nanoplates by UV-vis and by transmission electron microscopy (TEM) shows that there is a first stage where formation of 5 nm seeds takes place, further growth is probably by fusion and by direct reduction of gold onto the preformed nanoparticles. The nanoparticles formed during the photocatalytic reduction of the gold precursor show an irregular shape that evolves to regular triangular nanoplates after ripening in solution for 24 h.A photocatalytic approach was used to synthesize triangular nanoplates in aqueous solution. The synthesis is based on the reduction of a gold salt using a tin(iv) porphyrin as photocatalyst, cetyltrimethylammonium bromide (CTAB) as a stabilizing agent, and triethanolamine (TEA) as the final electron donor. The average edge length of the triangular nanoplates can be easily changed in the range 45-250 nm by varying the concentration of photocatalyst, and fine-tuning of the average edge length is achieved by varying the concentration of CTAB. Study of the mechanism of formation of the nanoplates by UV-vis and by transmission electron microscopy (TEM) shows that there is a first stage where formation of 5 nm seeds takes place, further growth is probably by fusion and by direct reduction of gold onto the preformed nanoparticles. The nanoparticles formed during the photocatalytic reduction of the gold precursor show an irregular shape that evolves to regular

  17. One-Pot Trimetallic Relay Catalysis: A Unified Approach for the Synthesis of β-Carbolines and Other [c]-Fused Pyridines.

    PubMed

    Dhiman, Seema; Mishra, Uttam K; Ramasastry, S S V

    2016-06-27

    A divergent strategy is presented for the synthesis of 1,3-di- and 1,3,4-trisubstituted β-carbolines through an unprecedented one-pot triple-orthogonal-metal relay catalysis, and 1,3-disubstituted 4-hydroxy-β-carbolines through a one-pot bimetallic relay catalysis from readily accessible 3-(2-aminophenyl)-5-hexenyn-3-ols. These strategies were elaborated to enable the synthesis of benzofuro[2,3-c]pyridines, benzothieno[2,3-c]pyridines, and isoquinolines, which otherwise require multistep synthesis.

  18. Synthesis of Quaternary Ammonium Salts of Tricyclic Cationic Drugs: A One-Pot Synthesis for the Bioorganic Chemistry Laboratory

    ERIC Educational Resources Information Center

    Brunauer, Linda S.; Mogannam, Abid C.; Hwee, Won B.; Chen, James Y.

    2007-01-01

    A one-pot conversion of tricyclic cationic drugs to their quaternary ammonium forms is described for a widely used bioactive drug: chlorpromazine, a phenothiazine-based antipsychotic. After conversion to its free base, the parent drug was methylated using substoichiometric amounts of methyl iodide dissolved in ether; the charged quaternary…

  19. One-pot synthesis of a gold nanoparticle-Vmh2 hydrophobin nanobiocomplex for glucose monitoring

    NASA Astrophysics Data System (ADS)

    Politi, Jane; De Stefano, Luca; Rea, Ilaria; Gravagnuolo, Alfredo Maria; Giardina, Paola; Methivier, Christophe; Casale, Sandra; Spadavecchia, Jolanda

    2016-05-01

    HydrophobinVmh2 is a small amphiphilic protein, which self-assembles on different surfaces and naturally interacts with glucose. Here, we report on the synthesis of a nanobiocomplex made of polyethylene glycol, Vmh2 and gold nanoparticles by a one-step process and on its ability to recognise glucose in an aqueous solution at 0.3-0.6-1.2 mg ml-1 concentrations. Even though the Vmh2 proteins are intrinsically bonded to the gold core, effective glucose interaction monitoring was demonstrated by using dynamic light scattering, ultraviolet-visible, polarization-modulated infrared reflection-absorption and x-ray photoelectron spectroscopies. Experimental results highlighted an affinity constant of 7.3 ± 0.3 mg ml-1 between the nanobiosystem and the sugar, and a detection sensitivity of 0.13 ± 0.06 a.u./mg ml-1.

  20. Size-Tunable Fe3O4 Spherical Nanoclusters Through a One-Pot Hydrothermal Synthesis.

    PubMed

    Leshuk, Timothy; Krishnakumar, Harish; Gu, Frank

    2015-07-01

    A new method is presented for the synthesis of monodisperse, size-tunable Fe3O4 spherical nanocluster particles through a simple, one-step hydrothermal reaction, according to a kinetics-controlled self-assembly process of smaller nanocrystals into hierarchical mesoporous aggregates. The mean diameter of the particles can be controlled over a broad range up to ~230 nm by simply varying the concentration of the precipitating reagent (urea or ammonia). The particles can be easily dispersed in water with excellent colloidal stability, exhibit a high surface area of ~ 60 m2 g(-1), and demonstrate size-dependent magnetic separation kinetics, where the larger nanoclusters exhibit rapid magnetophoresis, and the smaller nanoclusters remain inseparable. Thus particle size control is essential for improving magnetic separation processes.

  1. One pot sono-chemical synthesis of 2D layered MoS2 nanosheets

    NASA Astrophysics Data System (ADS)

    Kapatel, Sanni; Sumesh, C. K.

    2016-05-01

    Two-dimensional nanocrystals and monolayer of transition metal dichalcogenides show fascinating changes in its properties such as transition from direct to the indirect bandgap material. Due to light interaction with these monolayers optical absorption is enhanced in visible range a lot. Here, we report the synthesis of molybdenum disulphide (MoS2) nanocrystals through a time dependent sono-chemical liquid exfoliation method and its structural and optical analysis. The prepared nanocrystals of MoS2 have exhibited high crystalline quality with strong diffraction to the (002) plane at 14.44° in the X-ray diffractrogram. It was observed that the concentration of nanocrystals in the dispersion inclined by increasing the sonication time. The optical absorption study revealed an optical band gap of 1.84 eV.

  2. Zinc-oxide-silica-silver nanocomposite: Unique one-pot synthesis and enhanced catalytic and anti-bacterial performance.

    PubMed

    Kokate, Mangesh; Garadkar, Kalyanrao; Gole, Anand

    2016-12-01

    We describe herein a unique approach to synthesize zinc oxide-silica-silver (ZnO-SiO2-Ag) nanocomposite, in a simple, one-pot process. The typical process for ZnO synthesis by alkaline precipitation of zinc salts has been tweaked to replace alkali by alkaline sodium silicate. The free acid from zinc salts helps in the synthesis of silica nanoparticles, whereas the alkalinity of sodium silicate precipitates the zinc salts. Addition of silver ions into the reaction pot prior to addition of sodium silicate, and subsequent reduction by borohydride, gives additional functionality of metallic centres for catalytic applications. The synthesis strategy is based on our recent work typically involving acid-base type of cross-reactions and demonstrates a novel strategy to synthesize nanocomposites in a one-pot approach. Each component in the composite offers a unique feature. ZnO besides displaying mild catalytic and anti-bacterial behaviour is an excellent and a cheap 3-D support for heterogeneous catalysis. Silver nanoparticles enhance the catalytic & anti-bacterial properties of ZnO. Silica is an important part of the composite; which not only "glues" the two nanoparticles thereby stabilizing the nanocomposite, but also significantly enhances the surface area of the composite; which is an attractive feature of any catalyst composite. The nanocomposite is found to show excellent catalytic performance with very high turnover frequencies (TOFs) when studied for catalytic reduction of Rhodamine B (RhB) and 4-Nitrophenol (4-NP). Additionally, the composite has been tested for its anti-bacterial properties on three different bacterial strains i.e. E. coli, B. Cereus and Bacillus firmus. The mechanism for enhancement of catalytic performance has been probed by understanding the role of silica in offering accessibility to the catalyst via its porous high surface area network. The nanocomposite has been characterized by a host of different analytical techniques. The uniqueness of

  3. Zinc-oxide-silica-silver nanocomposite: Unique one-pot synthesis and enhanced catalytic and anti-bacterial performance.

    PubMed

    Kokate, Mangesh; Garadkar, Kalyanrao; Gole, Anand

    2016-12-01

    We describe herein a unique approach to synthesize zinc oxide-silica-silver (ZnO-SiO2-Ag) nanocomposite, in a simple, one-pot process. The typical process for ZnO synthesis by alkaline precipitation of zinc salts has been tweaked to replace alkali by alkaline sodium silicate. The free acid from zinc salts helps in the synthesis of silica nanoparticles, whereas the alkalinity of sodium silicate precipitates the zinc salts. Addition of silver ions into the reaction pot prior to addition of sodium silicate, and subsequent reduction by borohydride, gives additional functionality of metallic centres for catalytic applications. The synthesis strategy is based on our recent work typically involving acid-base type of cross-reactions and demonstrates a novel strategy to synthesize nanocomposites in a one-pot approach. Each component in the composite offers a unique feature. ZnO besides displaying mild catalytic and anti-bacterial behaviour is an excellent and a cheap 3-D support for heterogeneous catalysis. Silver nanoparticles enhance the catalytic & anti-bacterial properties of ZnO. Silica is an important part of the composite; which not only "glues" the two nanoparticles thereby stabilizing the nanocomposite, but also significantly enhances the surface area of the composite; which is an attractive feature of any catalyst composite. The nanocomposite is found to show excellent catalytic performance with very high turnover frequencies (TOFs) when studied for catalytic reduction of Rhodamine B (RhB) and 4-Nitrophenol (4-NP). Additionally, the composite has been tested for its anti-bacterial properties on three different bacterial strains i.e. E. coli, B. Cereus and Bacillus firmus. The mechanism for enhancement of catalytic performance has been probed by understanding the role of silica in offering accessibility to the catalyst via its porous high surface area network. The nanocomposite has been characterized by a host of different analytical techniques. The uniqueness of

  4. Zirconia-based catalyst for the one-pot synthesis of coumarin through Pechmann reaction

    NASA Astrophysics Data System (ADS)

    Khan, Shahid Ali; Khan, Sher Bahadar; Asiri, Abdullah M.; Ahmad, Ikram

    2016-07-01

    Coumarins play an important role in drug development with diverse biological applications. Herein, we present the synthesis of coumarin through Pechmann reaction by using zirconia-based heterogeneous catalysts (ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose) in a solvent-free condition at room temperature. ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose were identified through spectroscopic techniques such as FESEM, X-ray, EDS, XPS, and FT-IR. ZrO2-TiO2 showed the best catalytic performance while ZrO2/cellulose was inactive. The kinetic parameters were observed in a solvent-free condition as well as in toluene and ethanol. The temperature effect was extensively studied which revealed that increasing the temperature will increase the rate of reaction. The rate of reaction in a solvent-free condition, ethanol, and toluene were 1.7 × 10-3, 1.7 × 10-2, and 5.6 × 10-3 g mol-1 min-1, respectively.

  5. Zirconia-based catalyst for the one-pot synthesis of coumarin through Pechmann reaction.

    PubMed

    Khan, Shahid Ali; Khan, Sher Bahadar; Asiri, Abdullah M; Ahmad, Ikram

    2016-12-01

    Coumarins play an important role in drug development with diverse biological applications. Herein, we present the synthesis of coumarin through Pechmann reaction by using zirconia-based heterogeneous catalysts (ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose) in a solvent-free condition at room temperature. ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose were identified through spectroscopic techniques such as FESEM, X-ray, EDS, XPS, and FT-IR. ZrO2-TiO2 showed the best catalytic performance while ZrO2/cellulose was inactive. The kinetic parameters were observed in a solvent-free condition as well as in toluene and ethanol. The temperature effect was extensively studied which revealed that increasing the temperature will increase the rate of reaction. The rate of reaction in a solvent-free condition, ethanol, and toluene were 1.7 × 10(-3), 1.7 × 10(-2), and 5.6 × 10(-3) g mol(-1) min(-1), respectively.

  6. One pot synthesis and characterization of gold nanocatalyst using Sacha inchi (Plukenetia volubilis) oil: Green approach.

    PubMed

    Kumar, Brajesh; Smita, Kumari; Cumbal, Luis; Debut, Alexis

    2016-05-01

    In this report, a simple and cost-effective methodology has been developed to obtain gold nanoparticles (AuNPs) using Sacha inchi (Plukenetia volubilis) oil in the presence of sunlight. The spectroscopic and morphological properties of AuNPs were characterized by using UV-vis spectroscopy, transmission electron microscopy (TEM), particle size analyzer, and X-ray diffraction (XRD). UV-vis and TEM reveal that the nanostructure of the gold particles has surfaced plasmon resonance at 515-520nm and is almost spherical in shape with an average size of 5-15nm. XRD studies confirmed the face cubic center (fcc) unit cell structure of AuNPs. The as-synthesized AuNPs showed remarkable photocatalytic decomposition of the methylene blue (>75%) without using any reducing agent and weak antioxidant activity (21-16%) against 1,1-diphenyl-2-picrylhydrazyl at the different sunlight exposure times. The experimental approach is promising and suggested that the sunlight is a good source of energy for enhancement of AuNP synthesis via Sacha inchi oil and its photocatalytic activity.

  7. One pot synthesis and characterization of gold nanocatalyst using Sacha inchi (Plukenetia volubilis) oil: Green approach.

    PubMed

    Kumar, Brajesh; Smita, Kumari; Cumbal, Luis; Debut, Alexis

    2016-05-01

    In this report, a simple and cost-effective methodology has been developed to obtain gold nanoparticles (AuNPs) using Sacha inchi (Plukenetia volubilis) oil in the presence of sunlight. The spectroscopic and morphological properties of AuNPs were characterized by using UV-vis spectroscopy, transmission electron microscopy (TEM), particle size analyzer, and X-ray diffraction (XRD). UV-vis and TEM reveal that the nanostructure of the gold particles has surfaced plasmon resonance at 515-520nm and is almost spherical in shape with an average size of 5-15nm. XRD studies confirmed the face cubic center (fcc) unit cell structure of AuNPs. The as-synthesized AuNPs showed remarkable photocatalytic decomposition of the methylene blue (>75%) without using any reducing agent and weak antioxidant activity (21-16%) against 1,1-diphenyl-2-picrylhydrazyl at the different sunlight exposure times. The experimental approach is promising and suggested that the sunlight is a good source of energy for enhancement of AuNP synthesis via Sacha inchi oil and its photocatalytic activity. PMID:26945647

  8. Zirconia-based catalyst for the one-pot synthesis of coumarin through Pechmann reaction.

    PubMed

    Khan, Shahid Ali; Khan, Sher Bahadar; Asiri, Abdullah M; Ahmad, Ikram

    2016-12-01

    Coumarins play an important role in drug development with diverse biological applications. Herein, we present the synthesis of coumarin through Pechmann reaction by using zirconia-based heterogeneous catalysts (ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose) in a solvent-free condition at room temperature. ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose were identified through spectroscopic techniques such as FESEM, X-ray, EDS, XPS, and FT-IR. ZrO2-TiO2 showed the best catalytic performance while ZrO2/cellulose was inactive. The kinetic parameters were observed in a solvent-free condition as well as in toluene and ethanol. The temperature effect was extensively studied which revealed that increasing the temperature will increase the rate of reaction. The rate of reaction in a solvent-free condition, ethanol, and toluene were 1.7 × 10(-3), 1.7 × 10(-2), and 5.6 × 10(-3) g mol(-1) min(-1), respectively. PMID:27460593

  9. One-pot synthesis and antiproliferative activity of novel 2,4-diaminopyrimidine derivatives bearing piperidine and piperazine moieties.

    PubMed

    Ma, Wei-Feng; Yang, Hai-Kui; Hu, Meng-Jin; Li, Qian; Ma, Tian-Zhu; Zhou, Zhong-Zhen; Liu, Rui-Yuan; You, Wen-Wei; Zhao, Pei-Liang

    2014-09-12

    A series of novel 2,4-diaminopyrimidines containing piperidine and piperazine moieties were synthesized via an efficient one-pot methodology. The bioassay tests demonstrated that compounds 27 and 28 displayed much stronger antitumor activities against four human cancer cell lines (HepG2, A549, MDA-MB-231 and MCF-7) than positive control fluorouracil. Particularly, compound 28 showed a two-fold improvement compared to fluorouracil in inhibiting MDA-MB-231 and A549 cell proliferation with IC50 values of 7.46 and 12.78 μM, respectively. Further flow-activated cell sorting analysis revealed that the most promising compound 28 displayed a significant effect on G2/M cell-cycle arrest in a dose-dependent manner in MDA-MB-231 cells.

  10. One-pot synthesis of glycopolymer-porphyrin conjugate as photosensitizer for targeted cancer imaging and photodynamic therapy.

    PubMed

    Lu, Jiawei; Zhang, Weidong; Yuan, Lin; Ma, Wenjuan; Li, Xiao; Lu, Wei; Zhao, Yun; Chen, Gaojian

    2014-03-01

    One-pot system combining multi-reactions is used to synthesize novel porphyrin-glycopolymer conjugates. Sodium mercury amalgam is used to catalyze the reactions: 1) reduction of RAFT polymerized poly(2-(methacrylamido) glucopyranose) (PMAG), 2) converting protoporphyrin to protoporphyrinogen, 3) thiol-ene coupling reaction of PMAG and protoporphyrinogen. The product is oxidized in the same pot to generate the final porphyrin-PMAG conjugates. The resulting conjugates are characterized by NMR, GPC, UV-Vis, and fluorescence spectroscopy. Glycoparticles (≈ 200 nm) bearing glucose units are formed by dissolving the conjugates in water. Glycoparticles show enhanced binding ability toward Con A, bind K562 cells efficiently and kill these cells under light irradiation in dose and light treatment length dependent manners, illustrating the potential biological applications of the conjugates as photosensitizer for cancer imaging and photodynamic therapy.

  11. Facile, one-pot synthesis, and antibacterial activity of mesoporous silica nanoparticles decorated with well-dispersed silver nanoparticles.

    PubMed

    Tian, Yue; Qi, Juanjuan; Zhang, Wei; Cai, Qiang; Jiang, Xingyu

    2014-08-13

    In this study, we exploit a facile, one-pot method to prepare MCM-41 type mesoporous silica nanoparticles decorated with silver nanoparticles (Ag-MSNs). Silver nanoparticles with diameter of 2-10 nm are highly dispersed in the framework of mesoporous silica nanoparticles. These Ag-MSNs possess an enhanced antibacterial effect against both Gram-positive and Gram-negative bacteria by preventing the aggregation of silver nanoparticles and continuously releasing silver ions for one month. The cytotoxicity assay indicates that the effective antibacterial concentration of Ag-MSNs shows little effect on human cells. This report describes an efficient and economical route to synthesize mesoporous silica nanoparticles with uniform silver nanoparticles, and these nanoparticles show promising applications as antibiotics.

  12. Designation of highly efficient catalysts for one pot conversion of glycerol to lactic acid

    PubMed Central

    Tao, Meilin; Dan Zhang; Guan, Hongyu; Huang, Guohui; Wang, Xiaohong

    2016-01-01

    Production of lactic acid from glycerol is a cascade catalytic procedure using multifunctional catalysts combined with oxidative and acidic catalytic sites. Therefore, a series of silver-exchanged phosphomolybdic acid catalysts (AgxH3−xPMo12O40, x = 1 ~ 3, abbreviated as AgxPMo) was designed and applied in glycerol oxidation with O2 as an oxidant to produce lactic acid (LA) without adding any base. Among all, total silver exchanged phosphomolybdic acid (Ag3PMo) was found to be the most active one with LA selectivity of 93% at 99% conversion under mild conditions of 5 h at 60 °C. The exceptionally high efficiency was contributed to the generation of strong Lewis acid sites, enhanced redox potentials and water-tolerance. More importantly, Ag3PMo was tolerant in crude glycerol from biodiesel production. And the reaction mechanism was also discussed. Meanwhile, Ag3PMo acted as a heterogeneous catalyst for 12 recycles without loss of activity. PMID:27431610

  13. Designation of highly efficient catalysts for one pot conversion of glycerol to lactic acid

    NASA Astrophysics Data System (ADS)

    Tao, Meilin; Dan Zhang; Guan, Hongyu; Huang, Guohui; Wang, Xiaohong

    2016-07-01

    Production of lactic acid from glycerol is a cascade catalytic procedure using multifunctional catalysts combined with oxidative and acidic catalytic sites. Therefore, a series of silver-exchanged phosphomolybdic acid catalysts (AgxH3‑xPMo12O40, x = 1 ~ 3, abbreviated as AgxPMo) was designed and applied in glycerol oxidation with O2 as an oxidant to produce lactic acid (LA) without adding any base. Among all, total silver exchanged phosphomolybdic acid (Ag3PMo) was found to be the most active one with LA selectivity of 93% at 99% conversion under mild conditions of 5 h at 60 °C. The exceptionally high efficiency was contributed to the generation of strong Lewis acid sites, enhanced redox potentials and water-tolerance. More importantly, Ag3PMo was tolerant in crude glycerol from biodiesel production. And the reaction mechanism was also discussed. Meanwhile, Ag3PMo acted as a heterogeneous catalyst for 12 recycles without loss of activity.

  14. Expedient access to α,β-difunctionalized azepenes using α-halo eneformamides: application to the one-pot synthesis of 2-benzazepanes.

    PubMed

    Bassler, Daniel P; Spence, Laura; Alwali, Amir; Beale, Oliver; Beng, Timothy K

    2015-02-28

    The regioselective synthesis of α,β-difunctionalized (alkenyl, aryl, sulfonyl, allyl, or alkynyl) azepenes has been accomplished through α-halo eneformamides. A successful implementation of the vicinal functionalization strategy has led to a one-pot synthesis of 2-benzazepanes whose benzenoid portion is highly functionalized.

  15. A facile one-pot synthesis of colloidal stable, monodisperse, highly PEGylated CuS@mSiO2 nanocomposites for the combination of photothermal therapy and chemotherapy.

    PubMed

    Lu, Feng; Wang, Jinfeng; Yang, Lin; Zhu, Jun-Jie

    2015-06-11

    A facile one-pot approach was developed for the synthesis of colloidal stable, monodisperse, highly PEGylated mesoporous silica coated copper sulfide nanocomposites for the combination of photothermal therapy and chemotherapy. The proposed method can also be extended to the synthesis of other metal sulfide nanocomposites.

  16. Rapid Synthesis of Thiophene-Based, Organic Dyes for Dye-Sensitized Solar Cells (DSSCs) by a One-Pot, Four-Component Coupling Approach.

    PubMed

    Matsumura, Keisuke; Yoshizaki, Soichi; Maitani, Masato M; Wada, Yuji; Ogomi, Yuhei; Hayase, Shuzi; Kaiho, Tatsuo; Fuse, Shinichiro; Tanaka, Hiroshi; Takahashi, Takashi

    2015-06-26

    This one-pot, four-component coupling approach (Suzuki-Miyaura coupling/C-H direct arylation/Knoevenagel condensation) was developed for the rapid synthesis of thiophene-based organic dyes for dye-sensitized solar cells (DSSCs). Seven thiophene-based, organic dyes of various donor structures with/without the use of a 3,4-ethylenedioxythiophene (EDOT) moiety were successfully synthesized in good yields based on a readily available thiophene boronic acid pinacol ester scaffold (one-pot, 3-step, 35-61%). Evaluation of the photovoltaic properties of the solar cells that were prepared using the synthesized dyes revealed that the introduction of an EDOT structure beside a cyanoacrylic acid moiety improved the short-circuit current (Jsc) while decreasing the fill factor (FF). The donor structure significantly influenced the open-circuit voltage (Voc), the FF, and the power conversion efficiency (PCE). The use of a n-hexyloxyphenyl amine donor, and our originally developed, rigid, and nonplanar donor, both promoted good cell performance (η=5.2-5.6%).

  17. Superparamagnetic Au-Fe3O4 nanoparticles: one-pot synthesis, biofunctionalization and toxicity evaluation

    NASA Astrophysics Data System (ADS)

    Pariti, A.; Desai, P.; Maddirala, S. K. Y.; Ercal, N.; Katti, K. V.; Liang, X.; Nath, M.

    2014-09-01

    Superparamagnetic Au-Fe3O4 bifunctional nanoparticles have been synthesized using a single step hot-injection precipitation method. The synthesis involved using Fe(CO)5 as iron precursor and HAuCl4 as gold precursor in the presence of oleylamine and oleic acid. Oleylamine helps in reducing Au3+ to Au0 seeds which simultaneously oxidizes Fe(0) to form Au-Fe3O4 bifunctional nanoparticles. Triton® X-100 was employed as a highly viscous solvent to prevent agglomeration of Fe3O4 nanoparticles. Detailed characterization of these nanoparticles was performed by using x-ray powder diffraction, transmission electron microscopy, scanning tunneling electron microscopy, UV-visible spectroscopy, Mössbauer and magnetometry studies. To evaluate these nanoparticles’ applicability in biomedical applications, L-cysteine was attached to the Au-Fe3O4 nanoparticles and cytotoxicity of Au-Fe3O4 nanoparticles was tested using CHO cells by employing MTS assay. L-cysteine modified Au-Fe3O4 nanoparticles were qualitatively characterized using Fourier transform infrared spectroscopy and Raman spectroscopy; and quantitatively using acid ninhydrin assay. Investigations reveal that that this approach yields Au-Fe3O4 bifunctional nanoparticles with an average particle size of 80 nm. Mössbauer studies indicated the presence of Fe in Fe3+ in A and B sites (tetrahedral and octahedral, respectively) and Fe2+ in B sites (octahedral). Magnetic measurements also indicated that these nanoparticles were superparamagnetic in nature due to Fe3O4 region. The saturation magnetization for the bifunctional nanoparticles was observed to be ˜74 emu g-1, which is significantly higher than the previously reported Fe3O4 nanoparticles. Mössbauer studies indicated that there was no significant Fe(0) impurity that could be responsible for the superparamagnetic nature of these nanoparticles. None of the investigations showed any presence of other impurities such as Fe2O3 and FeOOH. These Au-Fe3O4 bifunctional

  18. One-pot, one-step, catalytic synthesis of 2,5-diformylfuran from fructose

    NASA Astrophysics Data System (ADS)

    Tao, Furong; Cui, Yuezhi; Yang, Pengfei; Gong, Yinghua

    2014-07-01

    MIL-101, a chromium-based metal-organic framework, is known for its very large pore size, large surface area and good stability. However, application of this material in catalysis is still limited. In this paper, a simple and practical catalytic method for the preparation 2,5-diformylfuran (DFF) directly from fructose was investigated. 5% Pd-V(3: 2)@MIL-101 was evaluated as a potential and effective catalyst for the direct oxidation of fructose. The amount of the catalyst, reaction time and temperature had a large effect on the reaction. At the optimized reaction conditions, when the reaction was conducted at 140°C for 600 min, 1 atm oxygen pressure, the yield of DFF reached 34%, fructose conversion was up to 100%. In our system, the main side products were 5-formyl-2-furancarboxylic acid (FFCA) and 2,5-furandicarboxylic acid (FDCA), which are the products of deep oxidation of DFF. This simple and effective catalytic system may be valuable to facilitate energy-efficient conversion of fructose into biofuels and platform chemicals.

  19. One-pot solvothermal synthesis of dual-phase titanate/titania Nanoparticles and their adsorption and photocatalytic Performances

    SciTech Connect

    Cheng, Yu Hua; Gong, Dangguo; Tang, Yuxin; Ho, Jeffery Weng Chye; Tay, Yee Yan; Lau, Wei Siew; Wijaya, Olivia; Lim, Jiexiang; Chen, Zhong

    2014-06-01

    Dual phase titanate/titania nanoparticles undergo phase transformation gradually with the increase of solvothermal synthesis temperature from 100 °C to 200 °C, and eventually are fully transformed into anatase TiO{sub 2}. The crystal structure change results in the changes of optical absorption, sensitizer/dopant formation and surface area of the materials which finally affect the overall dye removal ability. Reactions under dark and light have been conducted to distinguish the contributions of surface adsorption from photocatalytic degradation. The sample synthesized at 160 °C (S160) shows the best performances for both adsorption under dark and photocatalytic degradation of methylene blue (MB) under visible light irradiation. The adsorption mechanism for S160 is determined as monolayer adsorption based on the adsorption isotherm test under dark condition, and an impressive adsorption capacity of 162.19 mg/g is achieved. For the photocatalytic application, this sample at 0.1 g/L loading is also able to degrade 20 ppm MB within 6 hours under the visible light (>420 nm) condition. - Graphical abstract: The effect of solvothermal synthesis temperature on the formation and dye removal performance of dual phase titanate/titania nanoparticles was unveiled and optimized. - Highlights: • Low temperature one-pot solvothermal synthesis of dual-phase photocatalysts. • Correlation of the synthesis temperature is made with the phase composition. • Adsorption isotherm, kinetics, photocatalytic degradation were studied. • Synthesis at 160 °C yields the best material for adsorption of MB in dark. • The same sample also shows the best visible light degradation of MB.

  20. PdCo/Pd-Hexacyanocobaltate Hybrid Nanoflowers: Cyanogel-Bridged One-Pot Synthesis and Their Enhanced Catalytic Performance.

    PubMed

    Liu, Zhen-Yuan; Fu, Geng-Tao; Zhang, Lu; Yang, Xiao-Yu; Liu, Zhen-Qi; Sun, Dong-Mei; Xu, Lin; Tang, Ya-Wen

    2016-01-01

    Elaborate architectural manipulation of nanohybrids with multi-components into controllable 3D hierarchical structures is of great significance for both fundamental scientific interest and realization of various functionalities, yet remains a great challenge because different materials with distinct physical/chemical properties could hardly be incorporated simultaneously into the synthesis process. Here, we develop a novel one-pot cyanogel-bridged synthetic approach for the generation of 3D flower-like metal/Prussian blue analogue nanohybrids, namely PdCo/Pd-hexacyanocobaltate for the first time. The judicious introduction of polyethylene glycol (PEG) and the formation of cyanogel are prerequisite for the successful fabrication of such fascinating hierarchical nanostructures. Due to the unique 3D hierarchical structure and the synergistic effect between hybrid components, the as-prepared hybrid nanoflowers exhibit a remarkable catalytic activity and durability toward the reduction of Rhodamine B (RhB) by NaBH4. We expect that the obtained hybrid nanoflowers may hold great promises in water remediation field and beyond. Furthermore, the facile synthetic strategy presented here for synthesizing functional hybrid materials can be extendable for the synthesis of various functional hybrid nanomaterials owing to its versatility and feasibility. PMID:27573057

  1. A Facile Route for Patterned Growth of Metal-Insulator Carbon Lateral Junction through One-Pot Synthesis.

    PubMed

    Park, Beomjin; Park, Jaesung; Son, Jin Gyeong; Kim, Yong-Jin; Yu, Seong Uk; Park, Hyo Ju; Chae, Dong-Hun; Byun, Jinseok; Jeon, Gumhye; Huh, Sung; Lee, Seoung-Ki; Mishchenko, Artem; Hyun, Seung; Lee, Tae Geol; Han, Sang Woo; Ahn, Jong-Hyun; Lee, Zonghoon; Hwang, Chanyong; Novoselov, Konstantin S; Kim, Kwang S; Hong, Byung Hee; Kim, Jin Kon

    2015-08-25

    Precise graphene patterning is of critical importance for tailor-made and sophisticated two-dimensional nanoelectronic and optical devices. However, graphene-based heterostructures have been grown by delicate multistep chemical vapor deposition methods, limiting preparation of versatile heterostructures. Here, we report one-pot synthesis of graphene/amorphous carbon (a-C) heterostructures from a solid source of polystyrene via selective photo-cross-linking process. Graphene is successfully grown from neat polystyrene regions, while patterned cross-linked polystyrene regions turn into a-C because of a large difference in their thermal stability. Since the electrical resistance of a-C is at least 2 orders of magnitude higher than that for graphene, the charge transport in graphene/a-C heterostructure occurs through the graphene region. Measurement of the quantum Hall effect in graphene/a-C lateral heterostructures clearly confirms the reliable quality of graphene and well-defined graphene/a-C interface. The direct synthesis of patterned graphene from polymer pattern could be further exploited to prepare versatile heterostructures.

  2. PdCo/Pd-Hexacyanocobaltate Hybrid Nanoflowers: Cyanogel-Bridged One-Pot Synthesis and Their Enhanced Catalytic Performance

    PubMed Central

    Liu, Zhen-Yuan; Fu, Geng-Tao; Zhang, Lu; Yang, Xiao-Yu; Liu, Zhen-Qi; Sun, Dong-Mei; Xu, Lin; Tang, Ya-Wen

    2016-01-01

    Elaborate architectural manipulation of nanohybrids with multi-components into controllable 3D hierarchical structures is of great significance for both fundamental scientific interest and realization of various functionalities, yet remains a great challenge because different materials with distinct physical/chemical properties could hardly be incorporated simultaneously into the synthesis process. Here, we develop a novel one-pot cyanogel-bridged synthetic approach for the generation of 3D flower-like metal/Prussian blue analogue nanohybrids, namely PdCo/Pd-hexacyanocobaltate for the first time. The judicious introduction of polyethylene glycol (PEG) and the formation of cyanogel are prerequisite for the successful fabrication of such fascinating hierarchical nanostructures. Due to the unique 3D hierarchical structure and the synergistic effect between hybrid components, the as-prepared hybrid nanoflowers exhibit a remarkable catalytic activity and durability toward the reduction of Rhodamine B (RhB) by NaBH4. We expect that the obtained hybrid nanoflowers may hold great promises in water remediation field and beyond. Furthermore, the facile synthetic strategy presented here for synthesizing functional hybrid materials can be extendable for the synthesis of various functional hybrid nanomaterials owing to its versatility and feasibility. PMID:27573057

  3. One-pot one-cluster synthesis of fluorescent and bio-compatible Ag14 nanoclusters for cancer cell imaging.

    PubMed

    Yang, Jie; Xia, Nan; Wang, Xinan; Liu, Xianhu; Xu, An; Wu, Zhikun; Luo, Zhixun

    2015-11-28

    Small-molecule-protected silver nanoclusters have smaller hydrodynamic diameter, and thus may hold greater potential in biomedicine application compared with the same core-sized, macromolecule (i.e. DNA)-protected silver nanoclusters. However, the live cell imaging labeled by small-molecule-protected silver nanoclusters has not been reported until now, and the synthesis and atom-precise characterization of silver nanoclusters have been challenging for a long time. We develop a one-pot one-cluster synthesis method to prepare silver nanoclusters capped with GSH which is bio-compatible. The as-prepared silver nanoclusters are identified to be Ag14(SG)11 (abbreviated as Ag14, SG: glutathione) by isotope-resolvable ESI-MS. The structure is probed by 1D NMR spectroscopy together with 2D COSY and HSQC. This cluster species is fluorescent and the fluorescence quantum yield is solvent-dependent. Very importantly, Ag14 was successfully applied to label lung cancer cells (A549) for imaging, and this work represents the first attempt to image live cells with small-molecule-protected silver nanoclusters. Furthermore, it is revealed that the Ag14 nanoclusters exhibit lower cytotoxicity compared with some other silver species (including silver salt, silver complex and large silver nanoparticles), and the explanation is also provided. The comparison of silver nanoclusters to state-of-the-art labeling materials in terms of cytotoxicity and photobleaching lifetime is also conducted.

  4. A Facile Route for Patterned Growth of Metal-Insulator Carbon Lateral Junction through One-Pot Synthesis.

    PubMed

    Park, Beomjin; Park, Jaesung; Son, Jin Gyeong; Kim, Yong-Jin; Yu, Seong Uk; Park, Hyo Ju; Chae, Dong-Hun; Byun, Jinseok; Jeon, Gumhye; Huh, Sung; Lee, Seoung-Ki; Mishchenko, Artem; Hyun, Seung; Lee, Tae Geol; Han, Sang Woo; Ahn, Jong-Hyun; Lee, Zonghoon; Hwang, Chanyong; Novoselov, Konstantin S; Kim, Kwang S; Hong, Byung Hee; Kim, Jin Kon

    2015-08-25

    Precise graphene patterning is of critical importance for tailor-made and sophisticated two-dimensional nanoelectronic and optical devices. However, graphene-based heterostructures have been grown by delicate multistep chemical vapor deposition methods, limiting preparation of versatile heterostructures. Here, we report one-pot synthesis of graphene/amorphous carbon (a-C) heterostructures from a solid source of polystyrene via selective photo-cross-linking process. Graphene is successfully grown from neat polystyrene regions, while patterned cross-linked polystyrene regions turn into a-C because of a large difference in their thermal stability. Since the electrical resistance of a-C is at least 2 orders of magnitude higher than that for graphene, the charge transport in graphene/a-C heterostructure occurs through the graphene region. Measurement of the quantum Hall effect in graphene/a-C lateral heterostructures clearly confirms the reliable quality of graphene and well-defined graphene/a-C interface. The direct synthesis of patterned graphene from polymer pattern could be further exploited to prepare versatile heterostructures. PMID:26144549

  5. PdCo/Pd-Hexacyanocobaltate Hybrid Nanoflowers: Cyanogel-Bridged One-Pot Synthesis and Their Enhanced Catalytic Performance

    NASA Astrophysics Data System (ADS)

    Liu, Zhen-Yuan; Fu, Geng-Tao; Zhang, Lu; Yang, Xiao-Yu; Liu, Zhen-Qi; Sun, Dong-Mei; Xu, Lin; Tang, Ya-Wen

    2016-08-01

    Elaborate architectural manipulation of nanohybrids with multi-components into controllable 3D hierarchical structures is of great significance for both fundamental scientific interest and realization of various functionalities, yet remains a great challenge because different materials with distinct physical/chemical properties could hardly be incorporated simultaneously into the synthesis process. Here, we develop a novel one-pot cyanogel-bridged synthetic approach for the generation of 3D flower-like metal/Prussian blue analogue nanohybrids, namely PdCo/Pd-hexacyanocobaltate for the first time. The judicious introduction of polyethylene glycol (PEG) and the formation of cyanogel are prerequisite for the successful fabrication of such fascinating hierarchical nanostructures. Due to the unique 3D hierarchical structure and the synergistic effect between hybrid components, the as-prepared hybrid nanoflowers exhibit a remarkable catalytic activity and durability toward the reduction of Rhodamine B (RhB) by NaBH4. We expect that the obtained hybrid nanoflowers may hold great promises in water remediation field and beyond. Furthermore, the facile synthetic strategy presented here for synthesizing functional hybrid materials can be extendable for the synthesis of various functional hybrid nanomaterials owing to its versatility and feasibility.

  6. Inorganic-organic hybrid silica based tin complex as a novel, highly efficient and recyclable heterogeneous catalyst for the one-pot preparation of spirooxindoles in water.

    PubMed

    Ghahremanzadeh, Ramin; Rashid, Zahra; Zarnani, Amir-Hassan; Naeimi, Hossein

    2014-11-14

    In the present study, a tin complex immobilized on silica gel as a novel, green, highly efficient and heterogeneous reusable catalyst was synthesized by grafting 2-amino benzamide onto the silica gel surface as a result of the reaction between isatoic anhydride and 3-aminopropyl-functionalized silica gel, followed by complexing with tin chloride. The resulting organic-inorganic hybrid material was evaluated in the one-pot three-component synthesis of spiro[indoline-pyrazolo[4',3':5,6]pyrido[2,3-d]pyrimidine]trione derivatives in water via the condensation reaction of isatins, barbituric acids, and 1H-pyrazol-5-amines. All the reactions were completed in short reaction times and all the products were obtained in high to excellent yields with high purity. In addition, the synthesized novel catalyst could be separated from the reaction mixture by simple filtration and can be reused up to seven runs without significant loss in activity. PMID:25215454

  7. One-pot synthesis of iniferter-bound polystyrene core nanoparticles for the controlled grafting of multilayer shells

    NASA Astrophysics Data System (ADS)

    Marchyk, Nataliya; Maximilien, Jacqueline; Beyazit, Selim; Haupt, Karsten; Sum Bui, Bernadette Tse

    2014-02-01

    A novel approach using one-pot synthesis for the production of uniform, iniferter-bound polystyrene core nanoparticles of size 30-40 nm is described. Conventional oil-in-water emulsion polymerisation of styrene and divinylbenzene, combining a hybrid initiation system (thermal and UV), triggered sequentially, was employed to form the surface-bound thiocarbamate iniferters in situ. The iniferter cores were then used as seeds for re-initiating further polymerisation by UV irradiation to produce water-compatible core-shell nanoparticles. Grafting of various shell-types is demonstrated: linear polymers of poly(N-isopropylacrylamide) brushes, crosslinked polymers bearing different surface charges and molecularly imprinted polymers. The shell thickness was readily tuned by varying the monomers' concentration and polymerisation time. Our method is straightforward and in addition, gives access to the preparation of fluorescent seeds and the possibility of grafting nanosized multiple shells. The core-shell nanoparticles were fully characterised by dynamic light scattering, transmission electron microscopy, Fourier transform infrared spectroscopy and microelemental analysis.A novel approach using one-pot synthesis for the production of uniform, iniferter-bound polystyrene core nanoparticles of size 30-40 nm is described. Conventional oil-in-water emulsion polymerisation of styrene and divinylbenzene, combining a hybrid initiation system (thermal and UV), triggered sequentially, was employed to form the surface-bound thiocarbamate iniferters in situ. The iniferter cores were then used as seeds for re-initiating further polymerisation by UV irradiation to produce water-compatible core-shell nanoparticles. Grafting of various shell-types is demonstrated: linear polymers of poly(N-isopropylacrylamide) brushes, crosslinked polymers bearing different surface charges and molecularly imprinted polymers. The shell thickness was readily tuned by varying the monomers' concentration and

  8. β-Cyclodextrin-Propyl Sulfonic Acid Catalysed One-Pot Synthesis of 1,2,4,5-Tetrasubstituted Imidazoles as Local Anesthetic Agents.

    PubMed

    Ran, Yan; Li, Ming; Zhang, Zong-Ze

    2015-11-12

    Some functionalized 1,2,4,5-tetrasubstituted imidazole derivatives were synthesized using a one-pot, four component reaction involving 1,2-diketones, aryl aldehydes, ammonium acetate and substituted aromatic amines. The synthesis has been efficiently carried out in a solvent free medium using β-cyclodextrin-propyl sulfonic acid as a catalyst to afford the target compounds in excellent yields. The local anesthetic effect of these derivatives was assessed in comparison to lidocaine as a standard using a rabbit corneal and mouse tail anesthesia model. The three most potent promising compounds were subjected to a rat sciatic nerve block assay where they showed considerable local anesthetic activity, along with minimal toxicity. Among the tested analogues, 4-(1-benzyl-4,5-diphenyl-1H-imidazol-2-yl)-N,N-dimethylaniline (5g) was identified as most potent analogue with minimal toxicity. It was further characterized by a more favourable therapeutic index than the standard.

  9. β-Cyclodextrin-Propyl Sulfonic Acid Catalysed One-Pot Synthesis of 1,2,4,5-Tetrasubstituted Imidazoles as Local Anesthetic Agents.

    PubMed

    Ran, Yan; Li, Ming; Zhang, Zong-Ze

    2015-01-01

    Some functionalized 1,2,4,5-tetrasubstituted imidazole derivatives were synthesized using a one-pot, four component reaction involving 1,2-diketones, aryl aldehydes, ammonium acetate and substituted aromatic amines. The synthesis has been efficiently carried out in a solvent free medium using β-cyclodextrin-propyl sulfonic acid as a catalyst to afford the target compounds in excellent yields. The local anesthetic effect of these derivatives was assessed in comparison to lidocaine as a standard using a rabbit corneal and mouse tail anesthesia model. The three most potent promising compounds were subjected to a rat sciatic nerve block assay where they showed considerable local anesthetic activity, along with minimal toxicity. Among the tested analogues, 4-(1-benzyl-4,5-diphenyl-1H-imidazol-2-yl)-N,N-dimethylaniline (5g) was identified as most potent analogue with minimal toxicity. It was further characterized by a more favourable therapeutic index than the standard. PMID:26569210

  10. Ionic liquids as unique solvents in one-pot synthesis of 4-(n,2,2,2-tetranitroethylamino)-3-R-furazans.

    PubMed

    Sheremetev, Aleksei B; Aleksandrova, Nataly S; Palysaeva, Nadezhda V; Struchkova, Marina I; Tartakovsky, Vladimir A; Suponitsky, Kyrill Yu

    2013-09-01

    An efficient two-step one-pot protocol for the synthesis of N-nitrated trinitroethylamino furazans in an ionic liquid has been developed involving the condensation of aminofurazans with trinitroethanol and the N-nitration of an intermediate Mannich base. Trinitroethylnitramino derivatives have been synthesized and characterized by multinuclear NMR spectroscopy and X-ray crystallography. A role of the N,2,2,2-tetranitroethylamino group for stabilization of the high-density crystal-packing motif is described. The performance calculations gave detonation pressures and velocities for the furazan derivatives in a range of about 31-36 GPa and 8330-8745 ms(-1), respectively, which makes them competitive energetic materials. Furthermore, due to the positive oxygen balance, the compounds could be potential oxidizers for energetic formulations.

  11. One-pot template-free synthesis of porous CdMoO4 microspheres and their enhanced photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Madhusudan, Puttaswamy; Zhang, Jinfeng; Yu, Jiaguo; Cheng, Bei; Xu, Difa; Zhang, Jun

    2016-11-01

    The optical and catalytic performances of materials strongly depend on their size, morphology, dimensionality and structure. Herein, we demonstrate a facile one-pot template free synthesis of hierarchical CdMoO4 porous microspheres via a simple low temperature oil bath method. The photoactivity of the as-prepared samples was evaluated by photocatalytic decolorization of Methyl Orange (MO) and Methylene Blue (MB) mixed dye aqueous solutions at ambient temperature under full solar spectrum. The results indicated that the concentration of ammonium molybdate and reaction time greatly influence the diameter, average crystallite size, specific surface area, pore structure and photocatalytic activity of the prepared samples. Especially, under the suitable conditions the prepared hierarchical CdMoO porous microspheres exhibited enhanced photocatalytic activity and high stability. Furthermore, it is found that the photocatalytic activity and formation rate of hydroxyl radicals greatly depend on the particle sizes and morphology of as-prepared samples. This work not only demonstrates a simple way to fabricate the hierarchical CdMoO4 porous microspheres but also shows a possibility for utilization of CdMoO4 porous microspheres for the photocatalytic treatment of waste water pollutants.

  12. Low cost, surfactant-less, one pot synthesis of Cu{sub 2}O nano-octahedra at room temperature

    SciTech Connect

    Ahmed, Asar; Gajbhiye, Namdeo S.; Joshi, Amish G.

    2011-08-15

    Cu{sub 2}O octahedra were successfully synthesized via a novel wet-chemical method using D-glucose and hydrazine as reducing agent at room temperature without the presence of any other surfactant. Presence of D-glucose was important for the stabilization of the evolved copper octahedra and also for facilitating the reduction of the Cu(II) ions. The existence of glucose moieties on the surface as capping agent was confirmed by the FT-IR spectra while there was presence of excess oxygen atoms on the surface leading to the formation of a thin CuO layer at the octahedra surface, as confirmed by the XPS study, probably promoted by the capping glucose. Effect of NaOH concentration on the reaction and the formation of octahedra was also studied. The formation mechanism of obtained Cu{sub 2}O octahedra has been discussed. These octahedra were then studied for their photocatalytic properties in degradation of organic dyes, rhodamine B and methyl orange. - Graphical abstract: Cu{sub 2}O octahedra were found to have thin layer of CuO, due to oxidation of surface Cu{sup +} atoms by the surfactant O atoms. Highlights: > Simple and inexpensive one pot synthesis of various Cu{sub 2}O nanostructures. > Surface properties studied by XPS. > Used as photocatalysis for degradation of rhodamine B.

  13. One-pot synthesis of magnetite nanorods/graphene composites and its catalytic activity toward electrochemical detection of dopamine.

    PubMed

    Salamon, J; Sathishkumar, Y; Ramachandran, K; Lee, Yang Soo; Yoo, Dong Jin; Kim, Ae Rhan; Gnana Kumar, G

    2015-02-15

    Magnetite (Fe3O4) nanorods anchored over reduced graphene oxide (rGO) were synthesized through a one-pot synthesis method, where the reduction of GO and in-situ generation of Fe3O4 nanorods occurred concurrently. The average head and tail diameter of Fe3O4 nanorods anchored over the rGO matrix are found to be 32 and 11 nm, respectively, and morphology, structure and diameter of bare Fe3O4 nanorods were not altered even after the composite formation with rGO. The increased structural disorders and decrement in the sp(2) domains stimulated the high electrical conductivity and extended catalytic active sites for the prepared rGO/Fe3O4 nanocomposite. The constructed rGO/Fe3O4/GCE sensor exhibited excellent electrocatalytic activity toward the electrooxidation of dopamine (DA) with a quick response time of 6s, a wide linear range between 0.01 and 100.55 µM, high sensitivity of 3.15 µA µM(-1) cm(-2) and a lower detection limit of 7 nM. Furthermore, the fabricated sensor exhibited a practical applicability in the quantification of DA in urine samples with an excellent recovery rate. The excellent electroanalytical performances and straight-forward, surfactant and template free preparation method construct the rGO/Fe3O4 composite as an extremely promising material for the diagnosis of DA related diseases in biomedical applications.

  14. A One Pot Synthesis of Novel Bioactive Tri-Substitute-Condensed-Imidazopyridines that Targets Snake Venom Phospholipase A2

    PubMed Central

    Anilkumar, Nirvanappa C.; Sundaram, Mahalingam S.; Mohan, Chakrabhavi Dhananjaya; Rangappa, Shobith; Bulusu, Krishna C.; Fuchs, Julian E.; Girish, Kesturu S.; Bender, Andreas; Basappa; Rangappa, Kanchugarakoppal S.

    2015-01-01

    Drugs such as necopidem, saripidem, alpidem, zolpidem, and olprinone contain nitrogen-containing bicyclic, condensed-imidazo[1,2-α]pyridines as bioactive scaffolds. In this work, we report a high-yield one pot synthesis of 1-(2-methyl-8-aryl-substitued-imidazo[1,2-α]pyridin-3-yl)ethan-1-onefor the first-time. Subsequently, we performed in silico mode-of-action analysis and predicted that the synthesized imidazopyridines targets Phospholipase A2 (PLA2). In vitro analysis confirmed the predicted target PLA2 for the novel imidazopyridine derivative1-(2-Methyl-8-naphthalen-1-yl-imidazo [1,2-α]pyridine-3-yl)-ethanone (compound 3f) showing significant inhibitory activity towards snake venom PLA2 with an IC50 value of 14.3 μM. Evidently, the molecular docking analysis suggested that imidazopyridine compound was able to bind to the active site of the PLA2 with strong affinity, whose affinity values are comparable to nimesulide. Furthermore, we estimated the potential for oral bioavailability by Lipinski's Rule of Five. Hence, it is concluded that the compound 3f could be a lead molecule against snake venom PLA2. PMID:26196520

  15. One-pot, water-based and high-yield synthesis of tetrahedral palladium nanocrystal decorated graphene.

    PubMed

    Fu, Gengtao; Tao, Lin; Zhang, Min; Chen, Yu; Tang, Yawen; Lin, Jun; Lu, Tianhong

    2013-09-01

    This paper reports a facile, water-based and one-pot synthesis of tetrahedral Pd nanocrystals (Pd-TNPs) with high yield and good size monodispersity supported on reduced graphene oxide (RGO) nanosheets via a co-chemical reduction method. The key synthetic strategy employed a positively charged polyallylamine-Pd(II) complex (PAH-Pd(II)) with un-coordinated amine groups as a linker molecule to immobilize Pd(II) species on the negatively charged graphene oxide (GO) surface through electrostatic interaction. As characterized by transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), Raman spectroscopy, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) techniques, well-defined Pd-TNPs with an average size of 9 nm were uniformly distributed on the RGO surface. The as-prepared Pd-TNPs/RGO nanohybrid with excellent colloidal stability in aqueous solution exhibits superior catalytic activity towards the degradation of methylene blue (MB) compared to both unsupported Pd-TNPs and Pd black. Thus, the resultant Pd-TNPs/RGO nanohybrid, as a promising heterogeneous catalyst, might have wide potential applications in water-based catalysis systems for the future. PMID:23864026

  16. One-pot green hydrothermal synthesis of fluorescent nitrogen-doped carbon nanodots for in vivo bioimaging.

    PubMed

    Kuo, Tsung-Rong; Sung, Shuo-Yuan; Hsu, Chun-Wei; Chang, Chih-Jui; Chiu, Tai-Chia; Hu, Cho-Chun

    2016-01-01

    One-pot green synthesis of fluorescent nitrogen-doped carbon nanodots (CNDs) was developed by hydrothermal treatments of biocompatible polyvinylpyrrolidone (PVP) and glycine. The fluorescent nitrogen-doped CNDs exhibited excellent water solubility, low cytotoxicity, and good salt stability for biological imaging. UV-vis spectroscopy, fluorescence spectroscopy, transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) spectroscopy, and Raman spectroscopy were applied to confirm the optical and structural characteristics of the CNDs. Fluorescence of the CNDs was tunable from 417 to 450 nm adjusted by different excitation energy. Fluorescent quantum yield of the CNDs (21.43%) was significantly increased ~47.59% in comparison to that of the CNDs (14.52%) without nitrogen doping by glycine. In the in vivo imaging system (IVIS), fluorescence signal of the nitrogen-doped CNDs was obviously observed in the lungs at 12- and 24-h post-injection. Our work has shown the potential applications of the nitrogen-doped CNDs in fluorescence imaging in vivo.

  17. Controllable synthesis of hollow mesoporous silica particles by a facile one-pot sol-gel method.

    PubMed

    Song, Jing-Chuan; Xue, Fei-Fei; Lu, Zhong-Yuan; Sun, Zhao-Yan

    2015-07-01

    A simple and facile one-pot sol-gel method is proposed for the fabrication of hollow mesoporous silica particles. Both the particle size and the shell thickness can be well controlled by moderately tuning some experimental parameters.

  18. An efficient route for annulation of pyrimidines to steroids and non-steroids via a base catalyzed one-pot three component reaction.

    PubMed

    Saikia, Pallabi; Gogoi, Shyamalee; Gogoi, Sanjib; Boruah, Romesh C

    2014-10-01

    A facile strategy for the synthesis of steroidal A- and D-ring fused pyrimidines has been accomplished in high yields via a one-pot reaction of steroidal ketones, aromatic aldehydes and amidine derivatives in presence of potassium tert-butoxide in refluxing ethanol. The generality of the reaction was also extended to non-steroidal ketones.

  19. One-pot one-cluster synthesis of fluorescent and bio-compatible Ag14 nanoclusters for cancer cell imaging

    NASA Astrophysics Data System (ADS)

    Yang, Jie; Xia, Nan; Wang, Xinan; Liu, Xianhu; Xu, An; Wu, Zhikun; Luo, Zhixun

    2015-11-01

    Small-molecule-protected silver nanoclusters have smaller hydrodynamic diameter, and thus may hold greater potential in biomedicine application compared with the same core-sized, macromolecule (i.e. DNA)-protected silver nanoclusters. However, the live cell imaging labeled by small-molecule-protected silver nanoclusters has not been reported until now, and the synthesis and atom-precise characterization of silver nanoclusters have been challenging for a long time. We develop a one-pot one-cluster synthesis method to prepare silver nanoclusters capped with GSH which is bio-compatible. The as-prepared silver nanoclusters are identified to be Ag14(SG)11 (abbreviated as Ag14, SG: glutathione) by isotope-resolvable ESI-MS. The structure is probed by 1D NMR spectroscopy together with 2D COSY and HSQC. This cluster species is fluorescent and the fluorescence quantum yield is solvent-dependent. Very importantly, Ag14 was successfully applied to label lung cancer cells (A549) for imaging, and this work represents the first attempt to image live cells with small-molecule-protected silver nanoclusters. Furthermore, it is revealed that the Ag14 nanoclusters exhibit lower cytotoxicity compared with some other silver species (including silver salt, silver complex and large silver nanoparticles), and the explanation is also provided. The comparison of silver nanoclusters to state-of-the-art labeling materials in terms of cytotoxicity and photobleaching lifetime is also conducted.Small-molecule-protected silver nanoclusters have smaller hydrodynamic diameter, and thus may hold greater potential in biomedicine application compared with the same core-sized, macromolecule (i.e. DNA)-protected silver nanoclusters. However, the live cell imaging labeled by small-molecule-protected silver nanoclusters has not been reported until now, and the synthesis and atom-precise characterization of silver nanoclusters have been challenging for a long time. We develop a one-pot one

  20. Exfoliated Pd/HNb3O8 nanosheet as highly efficient bifunctional catalyst for one-pot cascade reaction

    NASA Astrophysics Data System (ADS)

    Lee, Nahaeng; Chung, Young-Min

    2016-05-01

    Ultrathin two-dimensional metal oxide nanosheets have drawn attention as potential solid acid catalysts owing to their strong acidity, attributed to the bridged OH groups formed on the nanosheets. In this study, a new class of bifunctional acid-metal catalyst was realized by the deposition of Pd on layered niobium oxide (KNb3O8 and HNb3O8) or its exfoliated nanosheet (Pd/HNb3O8-NS) and applied to one-pot cascade deacetalization and hydrogenation. It was found that the acid strength of the support exerted a large influence not only on the promotion of the first deacetalization step, but also on the acceleration of the subsequent hydrogenation step. Comparative experiments using a series of Pd/HZSM-5 catalysts with different acidities reconfirmed the crucial role of acid strength on hydrogenation. However, the superior catalytic activity of Pd/HNb3O8-NS for hydrogenation compared to that of Pd/HZSM-5 of similar acidity suggests a more efficient ensemble effect of the strong acid sites with the nearby metal sites on the nanosheet surface. Among the catalysts used, Pd/HNb3O8-NS showed the best catalytic performance for one-pot cascade reaction affording the desired product (benzyl alcohol) in approximately 92% yield, which was 7.1 and 1.2 times higher than that of layered Pd/KNb3O8 or Pd/HNb3O8, respectively. The excellent catalytic performance of Pd/HNb3O8-NS may result from the characteristic features of nanosheets: (i) the synergistic cooperation between the bifunctional active sites and (ii) the two-dimensional open surface offering easier access of the reactants to the active sites. Although the use of NaBH4 as hydrogen source was effective in improving the initial reaction performance, the basic nature of NaBH4 adversely resulted in weakening the acid strength of the catalyst, and consequently led to a reduction in catalytic activity.

  1. One-Pot Synthesis of Polysubstituted Spirofluorene-Indene via Ru(II)-Catalyzed [3 + 2] Annulation and Intramolecular Friedel-Crafts Cyclization.

    PubMed

    Zhu, Yu-Qin; Dong, Lin

    2015-10-16

    Ru(II)-catalyzed one-pot synthesis of polysubstituted spirofluorene-indenes via [3 + 2] annulation and then intramolecular Friedel-Crafts alkylation has been achieved. The simple method provides a broad scope of aryl ketones and internal alkynes, achieving PAHs skeletons in moderate to good yields. PMID:26419666

  2. Synthesis of unnatural amino acids via microwave-assisted regio-selective one-pot multi-component reactions of sulfamidates

    EPA Science Inventory

    Synthesis of triazole-based unnatural amino acids, triazole bisaminoacids and β-amino triazole has been described via stereo and regioselective one-pot multi-component reaction of sulfamidates, sodium azide, and alkynes under MW irradiation conditions. The developed method is app...

  3. Synthesis of β-arylated alkylamides via Pd-catalyzed one-pot installation of a directing group and C(sp3)–H arylation

    PubMed Central

    Zhang, Yi; Cao, Xiaoji; Wan, Jie-Ping

    2016-01-01

    Summary The synthesis of β-arylated alkylamides via alkyl C–H bond arylation has been realized by means of direct one-pot reactions of acyl chlorides, aryl iodides and 8-aminoquinoline. Depending on the structure of the starting materials, both single and double β-arylated alkylamides could be accessed. PMID:27340500

  4. Successively recycle waste as catalyst: a one-pot Wittig/1,4-reduction/Paal-Knorr sequence for modular synthesis of substituted furans.

    PubMed

    Chen, Long; Du, Yi; Zeng, Xing-Ping; Shi, Tao-Da; Zhou, Feng; Zhou, Jian

    2015-03-20

    A one-pot tandem Wittig/conjugate reduction/Paal-Knorr reaction is reported for the synthesis of di- or trisubstituted furans. This novel sequence first demonstrates the possibility of successively recycling waste from upstream steps to catalyze downstream reactions.

  5. Novel one pot synthesis of silver nanoparticle-polymer composites by supercritical CO2 polymerisation in the presence of a RAFT agent.

    PubMed

    Hasell, Tom; Thurecht, Kristofer J; Jones, Rhys D W; Brown, Paul D; Howdle, Steven M

    2007-10-14

    We report the one pot synthesis of a silver-polymer nanocomposite in supercritical carbon dioxide (scCO(2)) whereby an organometallic silver complex is thermally decomposed in the presence of a reversible addition fragmentation chain transfer (RAFT) agent during a polymerisation reaction in which the RAFT agent simultaneously stabilises the growing polymer microparticles and the formation of surface located silver nanoparticles.

  6. Synthesis of β-arylated alkylamides via Pd-catalyzed one-pot installation of a directing group and C(sp(3))-H arylation.

    PubMed

    Liu, Yunyun; Zhang, Yi; Cao, Xiaoji; Wan, Jie-Ping

    2016-01-01

    The synthesis of β-arylated alkylamides via alkyl C-H bond arylation has been realized by means of direct one-pot reactions of acyl chlorides, aryl iodides and 8-aminoquinoline. Depending on the structure of the starting materials, both single and double β-arylated alkylamides could be accessed.

  7. Manganese dioxide mediated one-pot synthesis of methyl 9H-pyrido[3,4-b]indole-1-carboxylate: Concise synthesis of alangiobussinine

    PubMed Central

    Baiget, Jessica; Llona-Minguez, Sabin; MacKay, Simon P; Suckling, Colin J; Sutcliffe, Oliver B

    2011-01-01

    Summary The carboline ring system is an important pharmacophore found in a number of biologically important targets. Development of synthetic routes for the preparation of these compounds is important in order to prepare a range of analogues containing the carboline heterocyclic moiety. A manganese dioxide mediated one-pot method starting with an activated alcohol and consisting of alcohol oxidation, Pictet–Spengler cyclisation, and oxidative aromatisation, offers a convenient process that allows access to β-carbolines. This one-pot process for the preparation of methyl 9H-pyrido[3,4-b]indole-1-carboxylate has subsequently been used as the key step in the synthesis of alangiobussinine and a closely related analogue. PMID:22043251

  8. Palladium-Catalyzed One-Pot Reaction of Hydrazones, Dihaloarenes, and Organoboron Reagents: Synthesis and Cytotoxic Activity of 1,1-Diarylethylene Derivatives.

    PubMed

    Roche, Maxime; Salim, Salim Mmadi; Bignon, Jérôme; Levaique, Hélène; Brion, Jean-Daniel; Alami, Mouad; Hamze, Abdallah

    2015-07-01

    A new three-component assembly reaction between N-tosylhydrazones, dihalogenated arenes, and boronic acids or boronate esters was developed, producing highly substituted 1,1-diarylethylenes in good yields. The two C-C bonds formed through this coupling have been catalyzed by a single Pd-catalyst in a one-pot fashion. It is noted that the one-pot pinacol boronate cross-coupling reaction generally provides products in high yields, offers an expansive substrate scope, and can address a broad range of aryl, styrene, vinyl, and heterocyclic olefinic targets. The scope of this one-pot coupling has been also extended to the synthesis of the 1,1-diarylethylene skeleton of the natural product ratanhine. The new compounds were evaluated for their cytotoxic activity, and this allowed the identification of compound 4ab that exhibits excellent antiproliferative activity in the nanomolar concentration range against HCT116 cancer cell lines. PMID:26036279

  9. Palladium-Catalyzed One-Pot Reaction of Hydrazones, Dihaloarenes, and Organoboron Reagents: Synthesis and Cytotoxic Activity of 1,1-Diarylethylene Derivatives.

    PubMed

    Roche, Maxime; Salim, Salim Mmadi; Bignon, Jérôme; Levaique, Hélène; Brion, Jean-Daniel; Alami, Mouad; Hamze, Abdallah

    2015-07-01

    A new three-component assembly reaction between N-tosylhydrazones, dihalogenated arenes, and boronic acids or boronate esters was developed, producing highly substituted 1,1-diarylethylenes in good yields. The two C-C bonds formed through this coupling have been catalyzed by a single Pd-catalyst in a one-pot fashion. It is noted that the one-pot pinacol boronate cross-coupling reaction generally provides products in high yields, offers an expansive substrate scope, and can address a broad range of aryl, styrene, vinyl, and heterocyclic olefinic targets. The scope of this one-pot coupling has been also extended to the synthesis of the 1,1-diarylethylene skeleton of the natural product ratanhine. The new compounds were evaluated for their cytotoxic activity, and this allowed the identification of compound 4ab that exhibits excellent antiproliferative activity in the nanomolar concentration range against HCT116 cancer cell lines.

  10. One-pot synthesis of hierarchical Cu2O/Cu hollow microspheres with enhanced visible-light photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Hong, Tianjie; Tao, Feifei; Lin, Jiudong; Ding, Wei; Lan, Mingxuan

    2015-08-01

    The hierarchical Cu2O/Cu hollow microspheres have been fabricated by the one-pot solvothermal redox method, which is one-step approach without any surfactant and template. By using the HRTEM, XRD, XPS and UV-vis spectroscopy, the as-prepared product is composed of Cu2O and Cu with energy band gap of 1.72 eV. Based on the time-dependent experiments, the content of Cu2O and Cu compositions can be effectively controlled by adjusting the reaction time and a possible mechanism is proposed. In addition, using various dye molecules to stimulate pollutants, the hierarchical Cu2O/Cu hollow microspheres reacted for 8 h exhibit excellent visible-light photocatalytic activities, which is much higher than those of the Cu2O/Cu catalysts formed at the shorter reaction time, commercial Cu2O powder and the mixture of alone Cu2O and Cu. This enhanced photocatalytic performance makes these hierarchical Cu2O/Cu hollow microspheres a kind of efficient visible-light photocatalyst in removing some organic compounds in wastewater.

  11. One-pot template-free synthesis of NaYF4 upconversion hollow nanospheres for bioimaging and drug delivery.

    PubMed

    Tian, Gan; Duan, Longsheng; Zhang, Xiao; Yin, Wenyan; Yan, Liang; Zhou, Liangjun; Liu, Xiaodong; Zheng, Xiaopeng; Li, Jinxia; Gu, Zhanjun; Zhao, Yuliang

    2014-06-01

    Hollow-structured nanomaterials with fluorescent properties are extremely attractive for image-guided cancer therapy. In this paper, sub-100 nm and hydrophilic NaYF4 upconversion (UC) hollow nanospheres (HNSs) with multicolor UC luminescence and drug-delivery properties were successfully prepared by a facile one-pot template-free hydrothermal route using polyetherimide (PEI) polymer as the stabilizing agent. XRD, SEM, TEM, and N2-adsorption/desorption were used to characterize the as-obtained products. The growth mechanism of the HNSs has been systematically investigated on the basis of the Ostwald ripening. Under 980 nm excitation, UC emissions of HNSs can be tuned by a simple change of the concentration or combination of various upconverters. As a result, the PEI-coated HNSs could be used as efficient probes for in vitro upconversion luminescence (UCL) cell imaging. Furthermore, a doxorubicin storage/release behavior and cancer-cell-killing ability investigation reveal that the product has the potential to be a drug carrier for cancer therapy.

  12. One-pot, three-component reaction using modified Julia reagents: a facile synthesis of 4,5-disubstituted 1,2,3-(NH)-triazoles in a wet organic solvent.

    PubMed

    Chai, Huihui; Guo, Ruiqiang; Yin, Wei; Cheng, Lingping; Liu, Renhua; Chu, Changhu

    2015-03-01

    A new one-pot, three component reaction involving the use of Julia reagent, aldehyde, and sodium azide was developed for the efficient synthesis of N-unsubstituted 1,2,3-triazoles. This reaction could be carried out under mild reaction conditions without any precaution, and broad scope of substrates, both respect to Julia reagents and aldehydes, could be applied in this reaction system in generation of a small library of title compounds.

  13. A facile one-pot sonochemical synthesis of surface-coated mannosyl protein microspheres for detection and killing of bacteria.

    PubMed

    Skirtenko, Natalia; Richman, Michal; Nitzan, Yeshayahu; Gedanken, Aharon; Rahimipour, Shai

    2011-12-01

    We report a remarkably facile one-pot sonochemical approach to prepare protein microspheres whose shells are covalently decorated with a mannosyl derivative to target Escherichia coli (E. coli), while their cores are encapsulated with tetracycline. Conjugated microspheres induced the agglutination of E. coli and increased the anti-bacterial activity of the encapsulated tetracycline by five fold.

  14. Facile one-pot synthesis of multi-yolk-shell Bi@C nanostructures by the nanoscale Kirkendall effect.

    PubMed

    Cui, C M; Guo, X H; Geng, Y M; Dang, T T; Xie, G; Chen, S P; Zhao, F Q

    2015-06-01

    Multi-yolk-shell Bi@C nanostructures were prepared via a facile one-pot template-free hydrothermal approach. The prepared Bi@C nanostructures can act as a solid catalyst in the thermal decomposition of cyclotrimethylenetrinitramine (RDX) and display excellent catalytic activity, which highlights their application in the field of energetic materials.

  15. One-pot Catalyst-free Synthesis of β- and γ-Hydroxy Sulfides Using Diaryliodonium Salts and Microwaves

    EPA Science Inventory

    A facile one-pot high-yield protocol is described for the preparation of β- and γ-hydroxy sulfides directly from diaryliodonium salts, potassium thiocyanate, and ethane-1,2-diol (ethylene glycol)/propane-1,3-diol (β-propylene glycol) without the need for any addit...

  16. One-Pot Catalyst-Free Synthesis of β- and γ-Hydroxy Sulfides using Diaryliodonium Salts and Microwave Irradiation

    EPA Science Inventory

    A facile one-pot high-yield protocol is described for the preparation of β- and γ-hydroxy sulfides directly from diaryliodonium salts, potassium thiocyanate, and ethane-1,2-diol (ethylene glycol)/propane-1,3-diol (β-propylene glycol) without the need for any additional catalyst o...

  17. Scalable One-pot Bacteria-templating Synthesis Route toward Hierarchical, Porous-Co3O4 Superstructures for Supercapacitor Electrodes

    PubMed Central

    Shim, Hyun-Woo; Lim, Ah-Hyeon; Kim, Jae-Chan; Jang, Eunjin; Seo, Seung-Deok; Lee, Gwang-Hee; Kim, T. Doohun; Kim, Dong-Wan

    2013-01-01

    Template-driven strategy has been widely used to synthesize inorganic nano/micro materials. Here, we used a bottom-up controlled synthesis route to develop a powerful solution-based method of fabricating three-dimensional (3D), hierarchical, porous-Co3O4 superstructures that exhibit the morphology of flower-like microspheres (hereafter, RT-Co3O4). The gram-scale RT-Co3O4 was facilely prepared using one-pot synthesis with bacterial templating at room temperature. Large-surface-area RT-Co3O4 also has a noticeable pseudocapacitive performance because of its high mass loading per area (~10 mg cm−2), indicating a high capacitance of 214 F g−1 (2.04 F cm−2) at 2 A g−1 (19.02 mA cm−2), a Coulombic efficiency averaging over 95%, and an excellent cycling stability that shows a capacitance retention of about 95% after 4,000 cycles. PMID:23900049

  18. One-pot solvothermal synthesis of a well-ordered layered sodium aluminoalcoholate complex: a useful precursor for the preparation of porous Al2O3 particles

    SciTech Connect

    Li, XS; Michaelis, VK; Ong, TC; Smith, SJ; McKay, I; Muller, P; Griffin, RG; Wang, EN

    2014-01-01

    One-pot solvothermal synthesis of a robust tetranuclear sodium hexakis(glycolato)tris(methanolato)aluminate complex Na-3[Al-4(OCH3)(3)(OCH2CH2O)(6)] via a modified yet rigorous base-catalyzed transesterification mechanism is presented here. Single crystal X-ray diffraction (SCXRD) studies indicate that this unique Al complex contains three pentacoordinate Al3+ ions, each bound to two bidentate ethylene glycolate chelators and one monodentate methanolate ligand. The remaining fourth Al3+ ion is octahedrally coordinated to one oxygen atom from each of the six surrounding glycolate chelators, effectively stitching the three pentacoordinate Al moieties together into a novel tetranuclear Al complex. This aluminate complex is periodically self-assembled into well-ordered layers normal to the [110] axis with the intra-/inter-layer bonding involving extensive ionic bonds from the three charge-counterbalancing Na+ cations rather than the more typical hydrogen bonding interactions as a result of fewer free hydroxyl groups present in its structure. It can also serve as a valuable precursor toward the facile synthesis of high-surface-area alumina powders using a very efficient rapid pyrolysis technique.

  19. One-pot synthesis of molecular bottle-brush functionalized single-walled carbon nanotubes with superior dispersibility in water.

    PubMed

    Deng, Yong; Hu, Qin; Yuan, Qiulin; Wu, Yan; Ling, Ying; Tang, Haoyu

    2014-01-01

    Molecular bottle-brush functionalized single-walled carbon nanotubes (SWCNTs) with superior dispersibility in water are prepared by a one-pot synthetic methodology. Elongating the main-chain and side-chain length of molecular bottle-brushes can further increase SWCNT dispersibility. They show significant enhancement of SWCNT dispersibility up to four times higher than those of linear molecular functionalized SWCNTs. PMID:24307218

  20. One-pot synthesis of tetracyclic fused imidazo[1,2-a]pyridines via a three-component reaction.

    PubMed

    Yang, Bo; Tao, Chuanye; Shao, Taofeng; Gong, Jianxian; Che, Chao

    2016-01-01

    A novel three-component reaction has been developed to assemble biologically and pharmaceutically important tetracyclic fused imidazo[1,2-a]pyridines in a one-pot fashion utilizing readily available 2-aminopyridines, isatins and isocyanides. The three-component coupling proceeds through the Groebke-Blackburn-Bienaymé reaction followed by a retro-aza-ene reaction and subsequent nucleophilic reaction of the in-situ generated imidazo[1,2-a]pyridines bearing an isocyanate functional group.

  1. Chemoenzymatic one-pot synthesis in an aqueous medium: combination of metal-catalysed allylic alcohol isomerisation-asymmetric bioamination.

    PubMed

    Ríos-Lombardía, Nicolás; Vidal, Cristian; Cocina, María; Morís, Francisco; García-Álvarez, Joaquín; González-Sabín, Javier

    2015-07-11

    The ruthenium-catalysed isomerisation of allylic alcohols was coupled, for the first time, with asymmetric bioamination in a one-pot process in an aqueous medium. In the cases involving prochiral ketones, the ω-TA exhibited excellent enantioselectivity, identical to that observed in the single step. As a result, amines were obtained from allylic alcohols with high overall yields and excellent enantiomeric excesses.

  2. One-pot green synthesis of reduced graphene oxide (RGO)/Fe3O4 nanocomposites and its catalytic activity toward methylene blue dye degradation

    NASA Astrophysics Data System (ADS)

    Vinothkannan, M.; Karthikeyan, C.; Gnana kumar, G.; Kim, Ae Rhan; Yoo, Dong Jin

    2015-02-01

    The reduced graphene oxide (RGO)/Fe3O4 nanocomposites were synthesized through a facile one-pot green synthesis by using solanum trilobatum extract as a reducing agent. Spherical shaped Fe3O4 nanoparticles with the diameter of 18 nm were uniformly anchored over the RGO matrix and the existence of fcc structured Fe3O4 nanoparticles over the RGO matrix was ensured from X-ray diffraction patterns. The amide functional groups exist in the solanum trilobatum extract is directly responsible for the reduction of Fe3+ ions and GO. The thermal stability of GO was increased by the removal of hydrophilic functional groups via solanum trilobatum extract and was further promoted by the ceramic Fe3O4 nanoparticles. The ID/IG ratio of RGO/Fe3O4 was increased over GO, indicating the extended number of structural defects and disorders in the RGO/Fe3O4 composite. The catalytic efficiency of prepared nanostructures toward methylene blue (MB) dye degradation mediated through the electron transfer process of BH4- ions was studied in detail. The π-π stacking, hydrogen bonding and electrostatic interaction exerted between the RGO/Fe3O4 composite and methylene blue, increased the adsorption efficiency of dye molecules and the large surface area and extended number of active sites completely degraded the MB dye within 12 min.

  3. One-pot synthesis of Cd1- x In x Te semiconductor as a sensitizer on TiO2 mesoporous for potential solar cell devices

    NASA Astrophysics Data System (ADS)

    Singsa-ngah, Mutika; Tubtimtae, Auttasit

    2015-08-01

    We demonstrated the synthesis of a new ternary semiconductor nanoparticle Cd1- x In x Te, as a sensitizer for solar cell devices via a one-pot mixed precursor solution. The Cd1- x In x Te nanoparticles (NPs) were prepared using the chemical bath deposition process and coated onto a TiO2 photoelectrode. A tetragonal structure of Cd1- x In x Te NPs was constituted on the TiO2 photoelectrode with a diameter range ˜25-30 nm, and the atomic percentages of the chemical elements showed that the structure could be Cd0.1In0.9Te incorporated with the CdIn2Te4 structure. When the dipping cycle increased, the energy gaps became narrower from 1.2 to 0.6 eV due to the increasing amount and the larger size of nanoparticles. The photovoltaic properties of various cycles were investigated, and the best power conversion efficiency ( η) of 0.49 % under full 1 sun illumination (100 mW/cm2, AM 1.5G) was obtained for the seven-cycle-Cd1- x In x Te NPs with a current density ( J sc) of 2.64 mA/cm2, an open-circuit voltage ( V oc) of 638 mV, and a fill factor ( FF) of 0.29. The efficiency of this material can be further improved for higher potential solar cell devices.

  4. One-pot synthesis of PEGylated plasmonic MoO(3-x) hollow nanospheres for photoacoustic imaging guided chemo-photothermal combinational therapy of cancer.

    PubMed

    Bao, Tao; Yin, Wenyan; Zheng, Xiaopeng; Zhang, Xiao; Yu, Jie; Dong, Xinghua; Yong, Yuan; Gao, Fuping; Yan, Liang; Gu, Zhanjun; Zhao, Yuliang

    2016-01-01

    Engineering design of plasmonic nanomaterials as on-demand theranostic nanoagents with imaging, drug carrier, and photothermal therapy (PTT) functions have profound impact on treatment of cancer. Here, a facile 'one-pot' template-free hydrothermal route was firstly developed for synthesis of plasmonic oxygen deficiency molybdenum oxide hollow nanospheres functionalized by poly(ethylene glycol) (PEG-MoO(3-x) HNSs). The as-prepared PEG-MoO(3-x) HNSs not only have good biocompatibility but also exhibit obvious localized surface plasmon resonance (LSPR) absorption in the near-infrared (NIR) region. Especially, due to its intrinsic mesoporous properties and effective photothermal conversion efficiency upon 808-nm NIR laser irradiation, the PEG-MoO(3-x) HNSs can be applied as a pH/NIR laser dual-responsive camptothecin (CPT) drug delivery nanoplatform for chemotherapy as well as PTT to cancer cells. A remarkably improved synergistic therapeutic effect to pancreatic (PANC-1) tumor-bearing mice was obtained compared to the result of chemotherapy or PTT alone. Apart from its application for drug delivery, the PEG-MoO(3-x) HNSs can also be employed as an effective contrast nanoagent for photoacoustic (PAT) imaging because of its high NIR absorption, making it promising as a theranostic nanoagent for PAT imaging-guided chemo-photothermal combinational cancer therapy in the nanomedicine field.

  5. One-Pot Aqueous Phase Synthesis of CdTe and CdTe/ZnS Core/Shell Quantum Dots.

    PubMed

    Zhou, Beiying; Yang, Fengjiu; Zhang, Xin; Cheng, Wenyan; Luo, Wei; Wang, Lianjun; Jiang, Wan

    2016-06-01

    A facile and economical one-pot strategy has been developed for the synthesis of water-solute CdTe and CdTe/ZnS core/shell quantum dots (QDs) using tellurium dioxide (TeO2) as a tellurium precursor and thioglycolic acid (TGA) as stabilizer without any pre-treatment and inert atmosphere protection. As-synthesized QDs were characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), electron diffraction spectroscopy (EDS), X-ray powder diffraction (XRD), UV-vis and photoluminescence (PL). The spherical particles were uniformly distributed with the average diameters of 3.2 nm (CdTe QDs) and -5 nm (CdTe/ZnS QDs). By altering the reaction conditions, the emission wavelengths of the CdTe core QDs and CdTe/ZnS core/shell QDs could be tuned from 508 to 574 nm and 526 to 600 nm with narrow full widths at half maximum (FWHM) of 33 to 58 nm, respectively. Meanwhile, on the optimum condition, the luminescence efficiency of CdTe/ZnS QDs can achieve to 74%, which was higher than that of CdTe core QDs (24%). PMID:27427627

  6. One-pot synthesis of quantum dot-labeled hydrophilic molecularly imprinted polymer nanoparticles for direct optosensing of folic acid in real, undiluted biological samples.

    PubMed

    Yang, Yaqiong; Wang, Zhengzheng; Niu, Hui; Zhang, Huiqi

    2016-12-15

    A facile and efficient one-pot approach for the synthesis of quantum dot (QD)-labeled hydrophilic molecularly imprinted polymer (MIP) nanoparticles for direct optosensing of folic acid (FA) in the undiluted bovine and porcine serums is described. Hydrophilic macromolecular chain transfer agent-mediated reversible addition-fragmentation chain transfer (RAFT) precipitation polymerization was used to implement the molecular imprinting of FA in the presence of CdTe quantum dots (QDs). The resulting FA-imprinted polymer nanoparticles with surface-grafted hydrophilic poly(glyceryl monomethacrylate) brushes and QDs labeling not only showed outstanding specific molecular recognition toward FA in biological samples, but also exhibited good photostability, rapid binding kinetics, and obvious template binding-induced fluorescence quenching. These characteristics make them a useful fluorescent chemosensor for directly and selectively optosensing FA in the undiluted bovine and porcine serums, with its limit of detection being 0.025μM and average recoveries ranging from 98% to 102%, even in the presence of several interfering compounds. This advanced fluorescent MIP chemosensor is highly promising for rapid quantification of FA in such applications as clinical diagnostics and food analysis. PMID:27453986

  7. A general and expeditious one-pot synthesis of sulfoxides in high optical purity from norephedrine-derived sulfamidites.

    PubMed

    García Ruano, José L; Alemparte, Carlos; Aranda, M Teresa; Zarzuelo, María M

    2003-01-01

    A general and simple procedure for preparing any kind of enantiomerically enriched sulfoxide starting from norephedrine-derived N-benzyloxycarbonylsulfamidite 3a is reported. After one-pot reaction of 3a with RMgX, HBF(4), and R'MgX, a variety of sulfoxides 6 are obtained in ee usually higher than 93% and isolated yields ranging between 50 and 78%. The obtained configuration is tunable by simply electing the order of the addition of the reagents. [reaction--see text

  8. One-pot synthesis of tetracyclic fused imidazo[1,2-a]pyridines via a three-component reaction.

    PubMed

    Yang, Bo; Tao, Chuanye; Shao, Taofeng; Gong, Jianxian; Che, Chao

    2016-01-01

    A novel three-component reaction has been developed to assemble biologically and pharmaceutically important tetracyclic fused imidazo[1,2-a]pyridines in a one-pot fashion utilizing readily available 2-aminopyridines, isatins and isocyanides. The three-component coupling proceeds through the Groebke-Blackburn-Bienaymé reaction followed by a retro-aza-ene reaction and subsequent nucleophilic reaction of the in-situ generated imidazo[1,2-a]pyridines bearing an isocyanate functional group. PMID:27559401

  9. Controlled silver delivery by silver-cellulose nanocomposites prepared by a one-pot green synthesis assisted by microwaves

    NASA Astrophysics Data System (ADS)

    Rosa Silva, Ana; Unali, Gianfranco

    2011-08-01

    Controlled silver release from cellulosic nanocomposites was achieved by synthesizing silver nanoparticles, under microwave heating for 1-15 min, in a one-pot, versatile and sustainable process in which microcrystalline cellulose simultaneously functions as reducing, stabilizing and supporting agent in water; chitin, starch and other cellulose derivatives could also be used as reducing, stabilizing and supporting agents for silver nanoparticles and the method was also found to be extensible to the preparation of noble metal (Au, Pt) and metal oxide nanoparticle (ZnO, Cu, CuO and Cu2O) nanocomposites.

  10. One-pot synthesis of fluorescent BSA-Ce/Au nanoclusters as ratiometric pH probes.

    PubMed

    Chen, Ya-Na; Chen, Po-Cheng; Wang, Chia-Wei; Lin, Yu-Shen; Ou, Chung-Mao; Ho, Lin-Chen; Chang, Huan-Tsung

    2014-08-11

    A facile, one-pot synthetic approach has been developed for the preparation of BSA-Ce/Au NCs. The fluorescence intensities of BSA-Ce/Au NCs at 410 and 650 nm are pH dependent and independent, respectively. The fluorescence intensity ratio (I410/I650) is linear against pH values from 6.0 to 9.0. These stable and biocompatible BSA-Ce/Au NCs have been used as ratiometric probes for monitoring local pH values inside HeLa cells.

  11. One-pot synthesis of tetracyclic fused imidazo[1,2-a]pyridines via a three-component reaction

    PubMed Central

    Yang, Bo; Tao, Chuanye; Shao, Taofeng

    2016-01-01

    Summary A novel three-component reaction has been developed to assemble biologically and pharmaceutically important tetracyclic fused imidazo[1,2-a]pyridines in a one-pot fashion utilizing readily available 2-aminopyridines, isatins and isocyanides. The three-component coupling proceeds through the Groebke–Blackburn–Bienaymé reaction followed by a retro-aza-ene reaction and subsequent nucleophilic reaction of the in-situ generated imidazo[1,2-a]pyridines bearing an isocyanate functional group. PMID:27559401

  12. Tetraethylene glycol promoted two-step, one-pot rapid synthesis of indole-3-[1-11C]acetic acid

    DOE PAGESBeta

    Lee, Sojeong; Qu, Wenchao; Alexoff, David L.; Shea, Colleen; Kim, Dohyun; Schueller, Michael; Fowler, Joanna S.

    2014-12-12

    An operationally friendly, two-step, one-pot process has been developed for the rapid synthesis of carbon-11 labeled indole-3-acetic acid ([11]IAA or [11]auxin). By replacing an aprotic polar solvent with tetraethylene glycol, nucleophilic [11]cyanation and alkaline hydrolysis reactions were performed consecutively in a single pot without a time-consuming intermediate purification step. The entire production time for this updated procedure is 55 min, which dramatically simplifies the entire synthesis and reduces the starting radioactivity required for a whole plant imaging study.

  13. Tetraethylene glycol promoted two-step, one-pot rapid synthesis of indole-3-[1-11C]acetic acid

    SciTech Connect

    Lee, Sojeong; Qu, Wenchao; Alexoff, David L.; Shea, Colleen; Kim, Dohyun; Schueller, Michael; Fowler, Joanna S.

    2014-12-12

    An operationally friendly, two-step, one-pot process has been developed for the rapid synthesis of carbon-11 labeled indole-3-acetic acid ([11]IAA or [11]auxin). By replacing an aprotic polar solvent with tetraethylene glycol, nucleophilic [11]cyanation and alkaline hydrolysis reactions were performed consecutively in a single pot without a time-consuming intermediate purification step. The entire production time for this updated procedure is 55 min, which dramatically simplifies the entire synthesis and reduces the starting radioactivity required for a whole plant imaging study.

  14. One-pot synthesis of co-substituted manganese oxide nanosheets and physical properties of lamellar aggregates

    SciTech Connect

    Kai, Kazuya; Cuisinier, Marine; Yoshida, Yukihiro; Saito, Gunzi; Kobayashi, Yoji; Kageyama, Hiroshi

    2012-11-15

    Graphical abstract: Display Omitted Highlights: ► Solid solution nanosheets, (Mn{sub 1−x}Co{sub x})O{sub 2}, synthesized via facile one-pot process. ► The structural characterization of nanosheets revealing a single (Mn,Co)O{sub 2} layer and the solubility limit as x ∼ 0.20. ► The invariant charge density of the layer upon Co substitution. ► Systematic dependence of magnetic and optical properties of the lamellar aggregates. -- Abstract: Co-substituted manganese oxide nanosheets, (Mn{sub 1−x}Co{sub x})O{sub 2} have been synthesized in the form of a colloidal suspension via a simple one-pot method. Substitution effects on the structural, optical absorption, and magnetic properties are investigated for the nanosheets and their lamellar aggregates. The composition of the (Mn{sub 1−x}Co{sub x})O{sub 2} nanosheets can be controlled continuously by adjusting the molar ratio of the starting materials. The solubility limit is x ∼ 0.20 based on the cell volume. In the 0.00 ≤ x ≤ 0.20 range, the band gap energy, magnetic moment, and Weiss temperature change systematically with x. The charge density of the (Mn,Co)O{sub 2} layer is independent of x (i.e., [(Mn,Co)O{sub 2}]{sup 0.2−}) and the cobalt ions are trivalent in low-spin state.

  15. One-pot hydrothermal synthesis of heterostructured ZnO/ZnS nanorod arrays with high ethanol-sensing properties.

    PubMed

    Gao, Peng; Wang, Longqiang; Wang, Ying; Chen, Yujin; Wang, Xiaona; Zhang, Guoli

    2012-04-10

    ZnO/ZnS heterostructured nanorod arrays with uniform diameter and length were synthesized from zinc substrates in a one-pot procedure by using a simple hydrothermal method. Structural characterization by HRTEM indicated that the heterostructured nanorods were composed of parallel segments of wurtzite-type ZnO and zinc-blende ZnS, with a distinct interface along the axial direction, which revealed the epitaxial relationship, ZnO (1010) and ZnS (111). The as-prepared ZnO/ZnS nanorods showed only two green emissions at around 523 nm and 576 nm. We also found that the nanorods exhibited high sensitivity to ethanol at relatively low temperatures, owing to their smaller size and structure.

  16. One-pot size and interior-cavity controlled synthesis of ZnO hollow micro-/nano-structured spheres.

    PubMed

    Yu, Yifei; Wang, Xi; Zhong, Yeteng; Zhang, Meng; Cao, Xinqiang; Zeng, Yi; Zheng, Jianyao; Ma, Ying; Yao, Jiannian

    2012-05-01

    In this work, ZnO hollow micro-/nano-structured microspheres were prepared via a one-pot solution route. The size and interior-cavity of these microspheres could be easily controlled by varying the precursor concentration. The hollow spherical assemblies were composed of short rod-like building units at low precursor concentration. When the precursor concentration increased, one-dimensional (1D) "pearl-chain-like" building units formed firstly and then self organized into hollow microspheres. The organization process and ripening of "pearl-chain-like" building units could be modulated by simply altering the reaction time. When tested in photocatalytic experiments, the hollow microspheres composed of loosely packed 1D "pearl-chain-like" building units showed higher activity than the densely packed ones. This method is very simple, mild, and may provide a new strategy to synthesize hierarchical self-assembled hollow structures.

  17. One-pot electrochemical synthesis of functionalized fluorescent carbon dots and their selective sensing for mercury ion.

    PubMed

    Hou, Yuxin; Lu, Qiujun; Deng, Jianhui; Li, Haitao; Zhang, Youyu

    2015-03-25

    We propose a simple, economical, and one-pot method to synthesize water-soluble functionalized fluorescent carbon dots (C-Dots) through electrochemical carbonization of sodium citrate and urea. The as-prepared C-Dots have good photostability and exhibit a high quantum yield of 11.9%. The sizes of the C-Dots are mainly distributed in the range of 1.0-3.5 nm with an average size of 2.4 nm. It has been further used as a novel label-free sensing probe for selective detection of Hg(2+) ions with detection limit as low as 3.3 nM. The detection linear range is 0.01-10 μM. The as-prepared C-Dots are also successfully applied for the determination of Hg(2+) in real water samples.

  18. One-pot synthesis and characterization of size-controlled bimagnetic FePt-iron oxide heterodimer nanocrystals.

    PubMed

    Figuerola, Albert; Fiore, Angela; Di Corato, Riccardo; Falqui, Andrea; Giannini, Cinzia; Micotti, Edoardo; Lascialfari, Alessandro; Corti, Maurizio; Cingolani, Roberto; Pellegrino, Teresa; Cozzoli, Pantaleo Davide; Manna, Liberato

    2008-01-30

    A one-pot, two-step colloidal strategy to prepare bimagnetic hybrid nanocrystals (HNCs), comprising size-tuned fcc FePt and inverse spinel cubic iron oxide domains epitaxially arranged in a heterodimer configuration, is described. The HNCs have been synthesized in a unique surfactant environment by temperature-driven sequential reactions, involving the homogeneous nucleation of FePt seeds and the subsequent heterogeneous growth of iron oxide. This self-regulated mechanism offers high versatility in the control of the geometric features of the resulting heterostructures, circumventing the use of more elaborate seeded growth techniques. It has been found that, as a consequence of the exchange coupling between the two materials, the HNCs exhibit tunable single-phase-like magnetic behavior, distinct from that of their individual components. In addition, the potential of the heterodimers as effective contrast agents for magnetic resonance imaging techniques has been examined.

  19. One-Pot Solvothermal Synthesis of Bi4V2O11 as A New Solar Water Oxidation Photocatalyst

    PubMed Central

    Jiang, Zaiyong; Liu, Yuanyuan; Li, Mengmeng; Jing, Tao; Huang, Baibiao; Zhang, Xiaoyang; Qin, Xiaoyan; Dai, Ying

    2016-01-01

    Bi4V2O11 was prepared via a one-pot solvothermal method and characterized via XRD, Raman, XPS, Electrochemical impedance spectroscopy. The as-prepared Bi4V2O11 sample displays excellent photocatalytic activity towards oxygen evolution under light irradiation. The hierarchical structure is in favour of the spatial separation of photogenerated electrons and holes. Furthermore, the internal polar field also plays a role in improving the charge separation. Both of the two results are responsible for excellent activity of O2 evolution. The resulting hierarchical Bi4V2O11 sample should be very promising photocatalyst for the application of photocatalytic O2 evolution in the future. PMID:26947126

  20. One-pot synthesis of disperse dyes under microwave irradiation: dyebath reuse in dyeing of polyester fabrics.

    PubMed

    Al-Etaibi, Alya M; El-Apasery, Morsy A; Mahmoud, Huda M; Al-Awadi, Nouria A

    2012-04-10

    A series of 4-hydroxyphenylazopyrazolopyrimidine disperse dyes were prepared via one-pot reactions of p-hydroxyphenylhydrazone, hydrazine hydrate, and acetylacetone or enaminones using microwave irradiation as an energy source. Structural assignments of the dyes were confirmed by X-ray crystallographic structure determination. Instead of discharging the dyebath after each dyeing cycle, the residual dyebath was spectrophotometrically analyzed and then pH readjusted for a repeat dyeing with longer time. Fastness of the dyed samples was measured after each recycle. Most of the dyed fabrics tested displayed good light fastness and excellent fastness to washing and perspiration. Finally, the biological activity of the synthesized dyes against Gram positive bacteria, Gram negative bacteria and yeast were evaluated.

  1. MOFs as multifunctional catalysts: one-pot synthesis of menthol from citronellal over a bifunctional MIL-101 catalyst.

    PubMed

    Cirujano, F G; Llabrés i Xamena, F X; Corma, A

    2012-04-14

    A bifunctional MOF catalyst containing coordinatively unsaturated Cr(3+) sites and palladium nanoparticles (Pd@MIL-101) has been used for the cyclization of citronellal to isopulegol and for the one-pot tandem isomerization/hydrogenation of citronellal to menthol. The MOF was found to be stable under the reaction conditions used, and the results obtained indicate that the performance of this bifunctional solid catalyst is comparable with other state-of-the-art materials for the tandem reaction: Full citronellal conversion was attained over Pd@MIL-101 in 18 h, with 86% selectivity to menthols and a diastereoselectivity of 81% to the desired (-)-menthol, while up to 30 h were necessary for attaining similar values over Ir/H-beta under analogous reaction conditions. PMID:22382815

  2. MOFs as multifunctional catalysts: one-pot synthesis of menthol from citronellal over a bifunctional MIL-101 catalyst.

    PubMed

    Cirujano, F G; Llabrés i Xamena, F X; Corma, A

    2012-04-14

    A bifunctional MOF catalyst containing coordinatively unsaturated Cr(3+) sites and palladium nanoparticles (Pd@MIL-101) has been used for the cyclization of citronellal to isopulegol and for the one-pot tandem isomerization/hydrogenation of citronellal to menthol. The MOF was found to be stable under the reaction conditions used, and the results obtained indicate that the performance of this bifunctional solid catalyst is comparable with other state-of-the-art materials for the tandem reaction: Full citronellal conversion was attained over Pd@MIL-101 in 18 h, with 86% selectivity to menthols and a diastereoselectivity of 81% to the desired (-)-menthol, while up to 30 h were necessary for attaining similar values over Ir/H-beta under analogous reaction conditions.

  3. One-pot green synthesis of 1,3,5-triarylpentane-1,5-dione and triarylmethane derivatives as a new class of tyrosinase inhibitors.

    PubMed

    Zheng, Zong-Ping; Zhang, Yi-Nan; Zhang, Shuang; Chen, Jie

    2016-02-01

    A new method was developed for one-pot green synthesis 1,3,5-triarylpentane-1,5-dione, triarylmethane, and flavonoid derivatives from the reaction between 2,4-dihydroxybenzaldehyde and hydroxyacetophenones via Aldol, Michael, and Friedel-Crafts additions using boric acid as catalyst in polyethylene glycol 400. The synthetic compounds demonstrated significant tyrosinase inhibitory activities much stronger than that of kojic acid. More important, 1,3,5-triarylpentane-1,5-dione and triarylmethane derivatives were found to be a new class of tyrosinase inhibitors. PMID:26754613

  4. Asymmetric, Three-Component, One-Pot Synthesis of Spiropyrazolones and 2,5-Chromenediones from Aldol Condensation/NHC-Catalyzed Annulation Reactions.

    PubMed

    Wang, Lei; Li, Sun; Chauhan, Pankaj; Hack, Daniel; Philipps, Arne R; Puttreddy, Rakesh; Rissanen, Kari; Raabe, Gerhard; Enders, Dieter

    2016-04-01

    A novel one-pot, three-component diastereo- and enantioselective synthesis of spiropyrazolones has been developed involving the aldol condensation of an enal to generate α,β-unsaturated pyrazolones, which react with a second equivalent of enal through an N-heterocyclic carbene (NHC)-catalyzed [3+2] annulation. The desired spirocyclopentane pyrazolones are obtained in moderate to good yields and good to excellent stereoselectivities. Alternatively, starting from cyclic 1,3-diketones, 2,5-chromenediones are available through [2+4] annulation.

  5. Activated alkene dependent one-pot, three-component aza-Morita-Baylis-Hillman reaction of ferrocenealdehyde: synthesis of highly functionalized diverse ferrocene derivatives.

    PubMed

    Madhavan, Suchithra; Shanmugam, Ponnusamy

    2011-04-01

    Activated alkene dependent one-pot, three-component aza-Morita-Baylis-Hillman (aza-MBH) reaction of ferrocenealdehyde afforded simple aza-MBH adduct of ferrocenealdehyde, unusual piperidine, β-amino acid residue, and γ-ketoester derivatives of ferrocene in good yield. The synthetic protocol with MVK has led to an unexpected ferrocenyl piperidine derivative in an excellent yield via diastereoselective domino aza-Michael/double Aldol pathway. Plausible mechanisms for the formation of unusual products and diastereoselectivity have also been described. The products can be used for the concise synthesis of ferrocenyl nitrogen heterocycles and bioconjugates.

  6. DABCO-catalyzed one-pot three component synthesis of dihydropyrano[3,2-c]chromene substituted quinazolines and their evaluation towards anticancer activity.

    PubMed

    Vodnala, Sumathi; Bhavani, A K D; Kamutam, Ramakrishna; Naidu, V G M; Promila; Prabhakar, Ch

    2016-08-15

    A facile DABCO promoted one-pot three component synthesis of a new series of C-C linked bis-heterocycle containing dihydropyrano[c]chromene as highly fused oxa-heteryl group at C-2 position of quinazoline was developed. Quinazoline-2-carbaldehyde, substituted 4-hydroxycoumarin and ethyl cyanoacetate were used as key components in the Knoevenagel-Michael addition reaction to get the titled compounds. These compounds were screened for anti-cancer activity against the breast cancer cell lines of MDA-MB 231, and MDA-MB 453. PMID:27432765

  7. Improved and optimized one-pot method for N-succinimidyl-4-[(18)F]fluorobenzoate ([(18)F]SFB) synthesis using microwaves.

    PubMed

    Li, Kang-Po; Hu, Ming-Kuan; Kwang-Fu Shen, Clifton; Lin, Wei-Yu; Hou, Shuang; Zhao, Li-Bo; Cheng, Cheng-Yi; Shen, Daniel H

    2014-12-01

    N-Succinimidyl-4-[(18)F]fluorobenzoate ([(18)F]SFB) is a potential prosthetic agent for novel tracer development in positron emission tomography (PET). Previously, we reported a microwave-assisted one-pot synthesis of [(18)F]SFB with high efficacy. Herein, we reveal an improved and optimized approach based on this former model for producing [(18)F]SFB. With optimized approaches, the entire protocol can be completed within 25min, and [(18)F]SFB is generated in satisfactory quality for direct use without further purification via high-performance liquid chromatography.

  8. One-pot wet-chemical co-reduction synthesis of bimetallic gold-platinum nanochains supported on reduced graphene oxide with enhanced electrocatalytic activity

    NASA Astrophysics Data System (ADS)

    Chen, De-Jun; Zhang, Qian-Li; Feng, Jin-Xia; Ju, Ke-Jian; Wang, Ai-Jun; Wei, Jie; Feng, Jiu-Ju

    2015-08-01

    In this work, a simple, rapid and facile one-pot wet-chemical co-reduction method is developed for synthesis of bimetallic Au-Pt alloyed nanochains supported on reduced graphene oxide (Au-Pt NCs/RGO), in which caffeine is acted as a capping agent and a structure-directing agent, while no any seed, template, surfactant or polymer involved. The as-prepared nanocomposites display enlarged electrochemical active surface area, significantly enhanced catalytic activity and better stability for methanol and ethylene glycol oxidation, compared with commercial Pt-C (Pt 50 wt%), PtRu-C (Pt 30 wt% and Ru 15 wt%) and Pt black.

  9. DABCO-catalyzed one-pot three component synthesis of dihydropyrano[3,2-c]chromene substituted quinazolines and their evaluation towards anticancer activity.

    PubMed

    Vodnala, Sumathi; Bhavani, A K D; Kamutam, Ramakrishna; Naidu, V G M; Promila; Prabhakar, Ch

    2016-08-15

    A facile DABCO promoted one-pot three component synthesis of a new series of C-C linked bis-heterocycle containing dihydropyrano[c]chromene as highly fused oxa-heteryl group at C-2 position of quinazoline was developed. Quinazoline-2-carbaldehyde, substituted 4-hydroxycoumarin and ethyl cyanoacetate were used as key components in the Knoevenagel-Michael addition reaction to get the titled compounds. These compounds were screened for anti-cancer activity against the breast cancer cell lines of MDA-MB 231, and MDA-MB 453.

  10. Asymmetric, Three-Component, One-Pot Synthesis of Spiropyrazolones and 2,5-Chromenediones from Aldol Condensation/NHC-Catalyzed Annulation Reactions.

    PubMed

    Wang, Lei; Li, Sun; Chauhan, Pankaj; Hack, Daniel; Philipps, Arne R; Puttreddy, Rakesh; Rissanen, Kari; Raabe, Gerhard; Enders, Dieter

    2016-04-01

    A novel one-pot, three-component diastereo- and enantioselective synthesis of spiropyrazolones has been developed involving the aldol condensation of an enal to generate α,β-unsaturated pyrazolones, which react with a second equivalent of enal through an N-heterocyclic carbene (NHC)-catalyzed [3+2] annulation. The desired spirocyclopentane pyrazolones are obtained in moderate to good yields and good to excellent stereoselectivities. Alternatively, starting from cyclic 1,3-diketones, 2,5-chromenediones are available through [2+4] annulation. PMID:26864437

  11. One-pot green synthesis of 1,3,5-triarylpentane-1,5-dione and triarylmethane derivatives as a new class of tyrosinase inhibitors.

    PubMed

    Zheng, Zong-Ping; Zhang, Yi-Nan; Zhang, Shuang; Chen, Jie

    2016-02-01

    A new method was developed for one-pot green synthesis 1,3,5-triarylpentane-1,5-dione, triarylmethane, and flavonoid derivatives from the reaction between 2,4-dihydroxybenzaldehyde and hydroxyacetophenones via Aldol, Michael, and Friedel-Crafts additions using boric acid as catalyst in polyethylene glycol 400. The synthetic compounds demonstrated significant tyrosinase inhibitory activities much stronger than that of kojic acid. More important, 1,3,5-triarylpentane-1,5-dione and triarylmethane derivatives were found to be a new class of tyrosinase inhibitors.

  12. One-Pot Synthesis of N-(α-Peroxy)Indole/Carbazole via Chemoselective Three-Component Condensation Reaction in Open Atmosphere.

    PubMed

    Wang, Xinbo; Pan, Yupeng; Huang, Kuo-Wei; Lai, Zhiping

    2015-11-20

    A facile one-pot synthesis of N-(α-peroxy)indole and N-(α-peroxy)carbazole has been developed using metal-free, organo-acid-catalyzed three-component condensation reactions of indole/carbazole, aldehyde, and peroxide. Based on the reaction discovered, a new synthetic proposal for Fumitremorgin A and Verruculogen is introduced. Such a protocol could be easily handled and scaled up in an open atmosphere with a wide substrate scope, enabling the construction of a new molecule library. PMID:26541059

  13. Synthesis and mechanism study of CdS quantum dots in two-phase liquid/liquid interfaces via one-pot route

    NASA Astrophysics Data System (ADS)

    Wang, Jidong; Guo, Kehong; Ke, Dandan; Han, Shumin

    2015-01-01

    The present letter reports a facile synthetic strategy in octadecene(ODE)/glycerol interfaces to prepare CdS quantum dots (QDs) with bright bandgap emission. In this synthesis, the precursors were not synthesized as a preceding step, but all chemicals were reacted simultaneously in a one-pot reaction. The monodispersed CdS QDs were synthesized in ODE/glycerol interfaces at 140, 160 and 180 °C, respectively. The thermodynamic equilibrium was proposed to explain the growth mechanism of CdS QDs in the ODE/glycerol interfaces.

  14. One-pot synthesis and control of aqueous soluble and organic soluble carbon dots from a designable waterborne polyurethane emulsion

    NASA Astrophysics Data System (ADS)

    Gu, Jiangjiang; Hu, Donghua; Huang, Jin; Huang, Xin; Zhang, Qiuhong; Jia, Xudong; Xi, Kai

    2016-02-01

    Carbon dots (CDs) have a wide range of applications and have drawn great interest in the recent decade. The fabrication and control of CDs with different solubilities are still urgent problems for their practical use. In this paper, aqueous soluble and organic soluble CDs (ACDs, OCDs) were produced by one-pot hydrothermal treatment of a designable waterborne polyurethane (WPU) emulsion. The difference in the solubility and fluorescence of these two kinds of CDs was attributed to the various functional groups on the surface, which were derived from the different segment fragments formed by hydrothermal treatment of a block polymer. It was found that the yields of the ACDs and OCDs could be regulated by means of selecting different soft segments in WPU. The more hydrophobic soft segments could result in an increase of the OCDs and a decrease of the ACDs. While the soft segments were hydrophilic or hydrolysable under hydrothermal conditions, only ACDs were obtained. The ACDs had good fluorescence and showed low cytotoxicity for use in multicolour bio-imaging. The OCDs processed good solubility in a wide range of organic solvents and were suitable for preparing fluorescent composite films with polymers.Carbon dots (CDs) have a wide range of applications and have drawn great interest in the recent decade. The fabrication and control of CDs with different solubilities are still urgent problems for their practical use. In this paper, aqueous soluble and organic soluble CDs (ACDs, OCDs) were produced by one-pot hydrothermal treatment of a designable waterborne polyurethane (WPU) emulsion. The difference in the solubility and fluorescence of these two kinds of CDs was attributed to the various functional groups on the surface, which were derived from the different segment fragments formed by hydrothermal treatment of a block polymer. It was found that the yields of the ACDs and OCDs could be regulated by means of selecting different soft segments in WPU. The more

  15. One-pot synthesis of hollow NiSe-CoSe nanoparticles with improved performance for hybrid supercapacitors

    NASA Astrophysics Data System (ADS)

    Chen, Haichao; Fan, Meiqiang; Li, Chao; Tian, Guanglei; Lv, Chunju; Chen, Da; Shu, Kangying; Jiang, Jianjun

    2016-10-01

    Hollow NiSe-CoSe samples have been synthesized for the first time via a one-pot solvothermal approach. The strategy is robust enough to synthesize NiSe-CoSe nanoparticles with different NiSe to CoSe ratios but with a similar hollow structure. Co ions in the NiSe-CoSe nanoparticles play decisive role for formation of the hollow structure; otherwise, the nanoparticles become solid for the NiSe sample. When used as the positive electroactive materials for energy storage, the NiSe-CoSe samples show excellent electrochemical activity in alkaline electrolyte. Using the synergistic effect between NiSe and CoSe, the electrochemical performance of NiSe-CoSe can be tuned by varying the NiSe to CoSe ratios. The NiSe-CoSe sample with a NiSe to CoSe ratio of 4:2 shows the best electrochemical performance in terms of superior specific capacity, improved rate capability and excellent cycling stability. In addition, the electrochemical performance of NiSe-CoSe sample with a NiSe to CoSe ratio of 4:2 is also evaluated via assembling hybrid supercapacitors with RGO, and the hybrid supercapacitor delivers both high power and energy densities (41.8 Wh kg-1 at 750 W kg-1 and 20.3 Wh kg-1 at 30 kW kg-1).

  16. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor.

    PubMed

    Jomma, Ezzaldeen Younes; Ding, Shou-Nian

    2016-01-01

    In this work, we presented a simple method to synthesize magnetite Prussian blue nano-composites (Fe₃O₄-PB) through one-pot hydrothermal process. Subsequently, the obtained nano-composites were used to fabricate a facile and effective glucose biosensor. The obtained nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, Fourier-transform infrared spectroscopy, UV-vis absorbance spectroscopy, cyclic voltammetry and chronoamperometry. The resultant Fe₃O₄-PB nanocomposites have magnetic properties which could easily controlled by an external magnetic field and the electro-catalysis of hydrogen peroxide. Thus, a glucose biosensor based on Fe₃O₄-PB was successfully fabricated. The biosensor showed super-electrochemical properties toward glucose detection exhibiting fast response time within 3 to 4 s, low detection limit of 0.5 µM and wide linear range from 5 µM to 1.2 mM with sensitivity of 32 µA∙mM(-1)∙cm(-2) and good long-term stability. PMID:26901204

  17. One pot synthesis and anti-biofilm potential of copper nanoparticles (CuNPs) against clinical strains of Pseudomonas aeruginosa.

    PubMed

    LewisOscar, Felix; MubarakAli, Davoodbasha; Nithya, Chari; Priyanka, Rajendran; Gopinath, Venkatraman; Alharbi, Naiyf S; Thajuddin, Nooruddin

    2015-01-01

    Pseudomonas aeruginosa, an opportunistic pathogen frequently associated with nosocomial infections, is emerging as a serious threat due to its resistance to broad spectrum antimicrobials. The biofilm mode of growth confers resistance to antibiotics and novel anti-biofilm agents are urgently needed. Nanoparticle based treatments and therapies have been of recent interest because of their versatile applications. This study investigates the anti-biofilm activity of copper nanoparticles (CuNPs) synthesized by the one pot method against P. aeruginosa. Standard physical techniques including UV-visible and Fourier transform infrared spectroscopy, X-ray diffraction and transmission electron microscopy were used to characterize the synthesized CuNPs. CuNP treatments at 100 ng ml(-1) resulted in a 94, 89 and 92% reduction in biofilm, cell surface hydrophobicity and exopolysaccharides respectively, without bactericidal activity. Evidence of biofilm inhibition was also seen with light and confocal microscope analysis. This study highlights the anti-biofilm potential of CuNPs, which could be utilized as coating agents on surgical devices and medical implants to manage biofilm associated infections.

  18. One-pot synthesis of interpenetrating inorganic/organic networks of CuO/resorcinol-formaldehyde aerogels: nanostructured energetic materials.

    PubMed

    Leventis, Nicholas; Chandrasekaran, Naveen; Sadekar, Anand G; Sotiriou-Leventis, Chariklia; Lu, Hongbing

    2009-04-01

    For many applications ranging from catalysis to sensors to energetic materials, it is desirable to produce intimate mixtures of nanoparticles. For instance, to improve the reaction rates of energetic materials, the oxidizing agent and the fuel need to be mixed as intimately as possible, ideally at the nanoscopic level. In this context, the acidity of a hydrated CuCl(2) solution reacting toward a network of CuO nanoparticles (a good oxidant) is used to induce one-pot cogelation of a nanostructured network of a resorcinol-formaldehyde resin (RF, the fuel). The resulting wet gels are dried to aerogels, and upon pyrolysis under Ar, the interpenetrating CuO/RF network undergoes a smelting reaction toward metallic Cu. Upon ignition in the open air, pure RF aerogels do not burn, while CuO/RF composites, even with substoichiometric CuO, sustain combustion, burning completely leaving only a solid residue of CuO whose role then has been that of a redox mediator through the smelting reaction.

  19. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor

    PubMed Central

    Jomma, Ezzaldeen Younes; Ding, Shou-Nian

    2016-01-01

    In this work, we presented a simple method to synthesize magnetite Prussian blue nano-composites (Fe3O4-PB) through one-pot hydrothermal process. Subsequently, the obtained nano-composites were used to fabricate a facile and effective glucose biosensor. The obtained nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, Fourier-transform infrared spectroscopy, UV-vis absorbance spectroscopy, cyclic voltammetry and chronoamperometry. The resultant Fe3O4-PB nanocomposites have magnetic properties which could easily controlled by an external magnetic field and the electro-catalysis of hydrogen peroxide. Thus, a glucose biosensor based on Fe3O4-PB was successfully fabricated. The biosensor showed super-electrochemical properties toward glucose detection exhibiting fast response time within 3 to 4 s, low detection limit of 0.5 µM and wide linear range from 5 µM to 1.2 mM with sensitivity of 32 µA∙mM−1∙cm−2 and good long-term stability. PMID:26901204

  20. A Facile One-Pot Synthesis of Au/Cu2O Nanocomposites for Nonenzymatic Detection of Hydrogen Peroxide

    NASA Astrophysics Data System (ADS)

    Chen, Ting; Tian, Liangliang; Chen, Yuan; Liu, Bitao; Zhang, Jin

    2015-06-01

    Au/Cu2O nanocomposites were successfully synthesized by a facile one-pot redox reaction without additional reducing agent under room temperature. The morphologies and structures of the as-prepared products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The electrocatalytic performance of Au/Cu2O nanocomposites towards hydrogen peroxide was evaluated by cyclic voltammetry (CV) and chronoamperometry (CA). The prepared Au/Cu2O nanocomposite electrode showed a wide linear range from 25 to 11.2 mM ( R = 0.9989) with a low detection limit of 1.05 μM ( S/ N = 3) and high sensitivity of 292.89 mA mM-1 cm-2. The enhanced performance for H2O2 detection can be attributed to the introduction of Au and the synergistic effect between Au and Cu2O. It is demonstrated that the Au/Cu2O nanocomposites material could be a promising candidate for H2O2 detection.

  1. One-pot, one-step synthesis of 2,5-diformylfuran from carbohydrates over Mo-containing Keggin heteropolyacids.

    PubMed

    Liu, Yu; Zhu, Liangfang; Tang, Jinqiang; Liu, Mingyang; Cheng, Ruodi; Hu, Changwei

    2014-12-01

    In this work, a one-pot strategy for directly converting fructose into 2,5-diformylfuran (DFF) over Mo-containing Keggin heteropolyacids (HPAs) in open air is developed. H3 PMo12 O40 HPA is found to show high activity and selectivity to the formation of DFF owing to its higher Brønsted acidity and moderate redox potential. The partial substitution of the H(+) in H3 PMo12 O40 with Cs(+) leads to the heterogenization of the HPA by forming its cesium salts Csx H3-x PMo12 (x=0.5, 1.5, and 2.5). A satisfactory yield of 69.3% to DFF is obtained over Cs0.5 H2.5 PMo12 polyoxometalate after deliberate optimization of the reaction conditions. The heterogenized polyoxometalate could be recycled and reused without significant loss of catalytic activity for five runs. The produced DFF could be separated from the resulting mixture by an adsorption-desorption method using activated carbon as the adsorbent and furfural as the desorbent. A highest isolated yield of 58.2% is obtained.

  2. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor.

    PubMed

    Jomma, Ezzaldeen Younes; Ding, Shou-Nian

    2016-01-01

    In this work, we presented a simple method to synthesize magnetite Prussian blue nano-composites (Fe₃O₄-PB) through one-pot hydrothermal process. Subsequently, the obtained nano-composites were used to fabricate a facile and effective glucose biosensor. The obtained nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, Fourier-transform infrared spectroscopy, UV-vis absorbance spectroscopy, cyclic voltammetry and chronoamperometry. The resultant Fe₃O₄-PB nanocomposites have magnetic properties which could easily controlled by an external magnetic field and the electro-catalysis of hydrogen peroxide. Thus, a glucose biosensor based on Fe₃O₄-PB was successfully fabricated. The biosensor showed super-electrochemical properties toward glucose detection exhibiting fast response time within 3 to 4 s, low detection limit of 0.5 µM and wide linear range from 5 µM to 1.2 mM with sensitivity of 32 µA∙mM(-1)∙cm(-2) and good long-term stability.

  3. One-pot synthesis of hybrid multifunctional silica nanoparticles with tunable coating by click chemistry in reverse w/o microemulsion.

    PubMed

    Tissandier, Cédric; Diop, Noël; Martini, Matteo; Roux, Stéphane; Tillement, Olivier; Hamaide, Thierry

    2012-01-10

    Multifunctional hybrid silica nanoparticles with a fluorescent core and tunable organic or polymeric shell can easily be prepared by a sol-gel process followed by 1,3 dipolar cycloaddition (CuAAC) in the same reverse quaternary W/O microemulsion. Compared to a classical multistep process, this one-pot synthesis reduces greatly the number of purification steps and avoids aggregation phenomena. The confinement of reactants inside the micellar system gives rise to a noticeable increase of the CuAAC reaction rate. In addition, using simultaneously two different substrates for CuAAC on silica allows us to obtain directly multifunctional hybrid nanoparticles displaying a double grafting without any separation or purification steps except the final recovery by centrifugation, which opens the door to a tunable coating of the nanoparticles. Particularly, the hydrophilic-lipophilic balance of the coating can be adjusted by implementing the pertinent MPEG:dodecyl azide ratio. As an application, the great versatility of this strategy has been proved by the one-pot synthesis of fluorescent silica nanoparticles with a PEG coating and encapsulating silver clusters. PMID:22066823

  4. A Practical One-Pot Synthesis of Positron Emission Tomography (PET) Tracers via Nickel-Mediated Radiofluorination

    PubMed Central

    Zlatopolskiy, Boris D; Zischler, Johannes; Urusova, Elizaveta A; Endepols, Heike; Kordys, Elena; Frauendorf, Holm; Mottaghy, Felix M; Neumaier, Bernd

    2015-01-01

    Recently a novel method for the preparation of 18F-labeled arenes via oxidative [18F]fluorination of easily accessible and sufficiently stable nickel complexes with [18F]fluoride under exceptionally mild reaction conditions was published. The suitability of this procedure for the routine preparation of clinically relevant positron emission tomography (PET) tracers, 6-[18F]fluorodopamine (6-[18F]FDA), 6-[18F]fluoro-l-DOPA (6-[18F]FDOPA) and 6-[18F]fluoro-m-tyrosine (6-[18F]FMT), was evaluated. The originally published base-free method was inoperative. However, a “low base” protocol afforded protected radiolabeled intermediates in radiochemical conversions (RCCs) of 5–18 %. The subsequent deprotection step proceeded almost quantitatively (>95 %). The simple one-pot two-step procedure allowed the preparation of clinical doses of 6-[18F]FDA and 6-[18F]FDOPA within 50 min (12 and 7 % radiochemical yield, respectively). In an unilateral rat model of Parkinsons disease, 6-[18F]FDOPA with high specific activity (175 GBq μmol−1) prepared using the described nickel-mediated radiofluorination was compared to 6-[18F]FDOPA with low specific activity (30 MBq μmol−1) produced via conventional electrophilic radiofluorination. Unexpectedly both tracer variants displayed very similar in vivo properties with respect to signal-to-noise ratio and brain distribution, and consequently, the quality of the obtained PET images was almost identical. PMID:26478840

  5. One-pot hydrothermal synthesis of Nitrogen-doped graphene as high-performance anode materials for lithium ion batteries

    PubMed Central

    Xing, Zheng; Ju, Zhicheng; Zhao, Yulong; Wan, Jialu; Zhu, Yabo; Qiang, Yinghuai; Qian, Yitai

    2016-01-01

    Nitrogen-doped (N-doped) graphene has been prepared by a simple one-step hydrothermal approach using hexamethylenetetramine (HMTA) as single carbon and nitrogen source. In this hydrothermal process, HMTA pyrolyzes at high temperature and the N-doped graphene subsequently self-assembles on the surface of MgO particles (formed by the Mg powder reacting with H2O) during which graphene synthesis and nitrogen doping are simultaneously achieved. The as-synthesized graphene with incorporation of nitrogen groups possesses unique structure including thin layer thickness, high surface area, mesopores and vacancies. These structural features and their synergistic effects could not only improve ions and electrons transportation with nanometer-scale diffusion distances but also promote the penetration of electrolyte. The N-doped graphene exhibits high reversible capacity, superior rate capability as well as long-term cycling stability, which demonstrate that the N-doped graphene with great potential to be an efficient electrode material. The experimental results provide a new hydrothermal route to synthesize N-doped graphene with potential application for advanced energy storage, as well as useful information to design new graphene materials. PMID:27184859

  6. Short one-pot chemo-enzymatic synthesis of L-lysine and L-alanine diblock co-oligopeptides.

    PubMed

    Fagerland, Jenny; Finne-Wistrand, Anna; Numata, Keiji

    2014-03-10

    Amphiphilic diblock co-oligopeptides are interesting and functional macromolecular materials for biomedical applications because of their self-assembling properties. Here, we developed a synthesis method for diblock co-oligopeptides by using chemo-enzymatic polymerization, which was a relatively short (30 min) and efficient reaction (over 40% yield). Block and random oligo(L-lysine-co-L-alanine) [oligo(Lys-co-Ala)] were synthesized using activated papain as enzymatic catalyst. The reaction time was optimized according to kinetic studies of oligo(L-alanine) and oligo(L-lysine). Using (1)H NMR spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, we confirmed that diblock and random co-oligopeptides were synthesized. Optical microscopy further revealed differences in the crystalline morphology between random and block co-oligopeptides. Plate-like, hexagonal, and hollow crystals were formed due to the strong impact of the monomer distribution and pH of the solution. The different crystalline structures open up interesting possibilities to form materials for both tissue engineering and controlled drug/gene delivery systems.

  7. One-pot synthesis of a new high vinyl content hybrid silica monolith dedicated to nanoliquid chromatography.

    PubMed

    Racha, El-Debs; Gay, Pauline; Dugas, Vincent; Demesmay, Claire

    2016-03-01

    A new vinyltrimethoxysilane-based hybrid silica monolith was developed and used as a reversed-phase capillary column. The synthesis of this rich vinyl hybrid macroporous monolith, by cocondensation of vinyltrimethoxysilane with tetramethoxysilane, was investigated using an unconventional (formamide, nitric acid) porogen/catalyst system. A macroporous hybrid silica monolith with 80% in mass of vinyltrimethoxysilane in the feeding silane solution was obtained and compared to a more conventional low vinyl content hybrid monolith with only of 20% vinyltrimethoxysilane. Monoliths were characterized by scanning electron microscopy, (29) Si nuclear magnetic resonance spectroscopy and N2 adsorption-desorption. About 80% of the vinyl precursor was incorporated in the final materials, leading to 15.9 and 61.5% of Si atoms bonded to vinyl groups for 20% vinyltrimethoxysilane and 80% vinyltrimethoxysilane, respectively. The 80% vinyltrimethoxysilane monolith presents a lower surface area than 20% vinyltrimethoxysilane (159 versus 551 m(2) /g), which is nevertheless compensated by a higher vinyl surface density. Chromatographic properties were evaluated in reversed-phase mode. Plots of ln(k) versus percentage of organic modifier were used to assess the reversed-phase mechanism. Its high content of organic groups leads to high retention properties. Column efficiencies of 170 000 plates/m were measured for this 80% vinyltrimethoxysilane hybrid silica monolith. Long capillary monolithic columns (90 cm) were successfully synthesized (N = 120 000).

  8. One-pot hydrothermal synthesis of Nitrogen-doped graphene as high-performance anode materials for lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Xing, Zheng; Ju, Zhicheng; Zhao, Yulong; Wan, Jialu; Zhu, Yabo; Qiang, Yinghuai; Qian, Yitai

    2016-05-01

    Nitrogen-doped (N-doped) graphene has been prepared by a simple one-step hydrothermal approach using hexamethylenetetramine (HMTA) as single carbon and nitrogen source. In this hydrothermal process, HMTA pyrolyzes at high temperature and the N-doped graphene subsequently self-assembles on the surface of MgO particles (formed by the Mg powder reacting with H2O) during which graphene synthesis and nitrogen doping are simultaneously achieved. The as-synthesized graphene with incorporation of nitrogen groups possesses unique structure including thin layer thickness, high surface area, mesopores and vacancies. These structural features and their synergistic effects could not only improve ions and electrons transportation with nanometer-scale diffusion distances but also promote the penetration of electrolyte. The N-doped graphene exhibits high reversible capacity, superior rate capability as well as long-term cycling stability, which demonstrate that the N-doped graphene with great potential to be an efficient electrode material. The experimental results provide a new hydrothermal route to synthesize N-doped graphene with potential application for advanced energy storage, as well as useful information to design new graphene materials.

  9. One-pot hydrothermal synthesis of Nitrogen-doped graphene as high-performance anode materials for lithium ion batteries.

    PubMed

    Xing, Zheng; Ju, Zhicheng; Zhao, Yulong; Wan, Jialu; Zhu, Yabo; Qiang, Yinghuai; Qian, Yitai

    2016-01-01

    Nitrogen-doped (N-doped) graphene has been prepared by a simple one-step hydrothermal approach using hexamethylenetetramine (HMTA) as single carbon and nitrogen source. In this hydrothermal process, HMTA pyrolyzes at high temperature and the N-doped graphene subsequently self-assembles on the surface of MgO particles (formed by the Mg powder reacting with H2O) during which graphene synthesis and nitrogen doping are simultaneously achieved. The as-synthesized graphene with incorporation of nitrogen groups possesses unique structure including thin layer thickness, high surface area, mesopores and vacancies. These structural features and their synergistic effects could not only improve ions and electrons transportation with nanometer-scale diffusion distances but also promote the penetration of electrolyte. The N-doped graphene exhibits high reversible capacity, superior rate capability as well as long-term cycling stability, which demonstrate that the N-doped graphene with great potential to be an efficient electrode material. The experimental results provide a new hydrothermal route to synthesize N-doped graphene with potential application for advanced energy storage, as well as useful information to design new graphene materials.

  10. One-pot hydrothermal synthesis of Nitrogen-doped graphene as high-performance anode materials for lithium ion batteries.

    PubMed

    Xing, Zheng; Ju, Zhicheng; Zhao, Yulong; Wan, Jialu; Zhu, Yabo; Qiang, Yinghuai; Qian, Yitai

    2016-01-01

    Nitrogen-doped (N-doped) graphene has been prepared by a simple one-step hydrothermal approach using hexamethylenetetramine (HMTA) as single carbon and nitrogen source. In this hydrothermal process, HMTA pyrolyzes at high temperature and the N-doped graphene subsequently self-assembles on the surface of MgO particles (formed by the Mg powder reacting with H2O) during which graphene synthesis and nitrogen doping are simultaneously achieved. The as-synthesized graphene with incorporation of nitrogen groups possesses unique structure including thin layer thickness, high surface area, mesopores and vacancies. These structural features and their synergistic effects could not only improve ions and electrons transportation with nanometer-scale diffusion distances but also promote the penetration of electrolyte. The N-doped graphene exhibits high reversible capacity, superior rate capability as well as long-term cycling stability, which demonstrate that the N-doped graphene with great potential to be an efficient electrode material. The experimental results provide a new hydrothermal route to synthesize N-doped graphene with potential application for advanced energy storage, as well as useful information to design new graphene materials. PMID:27184859

  11. One-pot synthesis of silicon nanoparticles trapped in ordered mesoporous carbon for use as an anode material in lithium-ion batteries.

    PubMed

    Park, Junsu; Kim, Gil-Pyo; Nam, Inho; Park, Soomin; Yi, Jongheop

    2013-01-18

    Silicon nanoparticles trapped in an ordered mesoporous carbon composite were prepared by a one-step self-assembly with solvent evaporation using the triblock copolymer Pluronic F127 and a resorcinol-formaldehyde polymer as the templating agent and carbon precursor respectively. Such a one-pot synthesis of Si/ordered mesoporous carbon nanocomposite is suitable for large-scale synthesis. Characterization confirmed that the Si nanoparticles were trapped in the ordered mesoporous carbon, as evidenced by transmission electron microscopy, x-ray diffraction analysis and nitrogen sorption isotherms. The composite showed a high reversible capacity above 700 mA h g(-1) during 50 cycles at 2 A g(-1). The improved electrochemical performance of the composite can be ascribed to the buffering effect of spaces formed in the ordered pore channels during the volume expansion of silicon and the rapid movement of lithium ions through the uniform cylindrical pore structure of the mesopores.

  12. One-pot synthesis of silicon nanoparticles trapped in ordered mesoporous carbon for use as an anode material in lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Park, Junsu; Kim, Gil-Pyo; Nam, Inho; Park, Soomin; Yi, Jongheop

    2013-01-01

    Silicon nanoparticles trapped in an ordered mesoporous carbon composite were prepared by a one-step self-assembly with solvent evaporation using the triblock copolymer Pluronic F127 and a resorcinol-formaldehyde polymer as the templating agent and carbon precursor respectively. Such a one-pot synthesis of Si/ordered mesoporous carbon nanocomposite is suitable for large-scale synthesis. Characterization confirmed that the Si nanoparticles were trapped in the ordered mesoporous carbon, as evidenced by transmission electron microscopy, x-ray diffraction analysis and nitrogen sorption isotherms. The composite showed a high reversible capacity above 700 mA h g-1 during 50 cycles at 2 A g-1. The improved electrochemical performance of the composite can be ascribed to the buffering effect of spaces formed in the ordered pore channels during the volume expansion of silicon and the rapid movement of lithium ions through the uniform cylindrical pore structure of the mesopores.

  13. Solid catalysts for multistep reactions: one-pot synthesis of 2,3-dihydro-1,5-benzothiazepines with solid acid and base catalysts.

    PubMed

    Climent, Maria J; Corma, Avelino; Iborra, Sara; Martí, Laura

    2014-04-01

    1,5-Benzothiazepines derivatives were obtained first by starting from 1,3-diphenylpropenone derivatives (chalcones) and 2-aminothiophenol by using aluminosilicate solid catalysts. However, diffusional limitations and the strong adsorption of products on the catalyst are deleterious for catalyst activity and life. Then a structured amorphous mesoporous catalyst with large pores and mild acidity that works at higher temperatures allowed us to obtain high conversions (99 %) and selectivities (98 %) of the desired product. A one-pot synthesis of 1,5-benzothiazepines that starts from benzaldehyde, acetophenone, and 2-aminothiophenol with 95 % yield was performed by combining optimized solid base and acid catalysts in batch mode as well as in a continuous-flow reactor system. Much better conversion and selectivity as well as process intensification has been achieved with the structured mesoporous materials by avoiding intermediate and final neutralization and purification steps required in the synthesis reported previously that uses homogeneous catalysts.

  14. Microwave-assisted one-pot synthesis of ring-fused aminals under catalyst- and solvent-free conditions

    EPA Science Inventory

    Heterocyclic compounds hold a special place in drug discovery and variety of techniques such as combinatorial synthesis, parallel synthesis, and automated library production to increase the output of these entities has been developed. Although most of these techniques are rapid a...

  15. Ag2Te quantum dots with compact surface coatings of multivalent polymers: ambient one-pot aqueous synthesis and the second near-infrared bioimaging.

    PubMed

    Yang, Min; Gui, Rijun; Jin, Hui; Wang, Zonghua; Zhang, Feifei; Xia, Jianfei; Bi, Sai; Xia, Yanzhi

    2015-02-01

    In this study, we described a facile ambient one-pot aqueous synthesis of fluorescent Ag2Te quantum dots (QDs) adopting multivalent polymers (poly(maleic anhydride) homopolymers) as stabilizers. In experiments, Ag2Te QDs were synthesized via a stepwise addition of the stabilizers, precursors (AgNO3/Na2TeO3) and promoters (NaBH4/N2H4 · H2O) in ambient one-pot aqueous solution. By regulating the compositions of raw materials, water-dispersed Ag2Te QDs (3.8-4.7 nm) were achieved and exhibited tunable photoluminescence (PL) emission (995-1068 nm) in the second near-infrared (NIR-II) region, accompanying with the minimized surface coating thickness (1.5-1.9 nm). Such compact coating of multivalent polymers promoted PL emission of Ag2Te QDs, so showing high PL quantum yields (PLQYs: 13.1-15.2%). In addition to compact sizes and high PLQYs, experimental results testified that the Ag2Te QDs demonstrated high photo-/colloidal stability and ultralow cytotoxicity, which implied their promising applications, especially serving as an effective nanoprobe for bioimaging in the NIR-II biological window.

  16. A Fully-automated One-pot Synthesis of [18F]Fluoromethylcholine with Reduced Dimethylaminoethanol Contamination via [18F]Fluoromethyl Tosylate

    PubMed Central

    Rodnick, Melissa E.; Brooks, Allen F.; Hockley, Brian G.; Henderson, Bradford D.; Scott, Peter J. H.

    2013-01-01

    Introduction A novel one-pot method for preparing [18F]fluoromethylcholine ([18F]FCH) via in situ generation of [18F]fluoromethyl tosylate ([18F]FCH2OTs), and subsequent [18F]fluoromethylation of dimethylaminoethanol (DMAE), has been developed. Methods [18F]FCH was prepared using a GE TRACERlab FXFN, although the method should be readily adaptable to any other fluorine-18 synthesis module. Initially ditosylmethane was fluorinated to generate [18F]FCH2OTs. DMAE was then added and the reaction was heated at 120°C for 10 min to generate [18F]FCH. After this time, reaction solvent was evaporated, and the crude reaction mixture was purified by solid-phase extraction using C18-Plus and CM-Light Sep-Pak cartridges to provide [18F]FCH formulated in USP saline. The formulated product was passed through a 0.22 μm filter into a sterile dose vial, and submitted for quality control testing. Total synthesis time was 1.25 hours from end-of-bombardment. Results Typical non-decay-corrected yields of [18F]FCH prepared using this method were 91 mCi (7% non-decay corrected based upon ~1.3 Ci [18F]fluoride), and doses passed all other quality control (QC) tests. Conclusion A one-pot liquid-phase synthesis of [18F]FCH has been developed. Doses contain extremely low levels of residual DMAE (31.6 μg / 10 mL dose or ~3 ppm) and passed all other requisite QC testing, confirming their suitability for use in clinical imaging studies. PMID:23665261

  17. Size-controlled one-pot synthesis of fluorescent cadmium sulfide semiconductor nanoparticles in an apoferritin cavity.

    PubMed

    Iwahori, K; Yamashita, I

    2008-12-10

    A simple size-controlled synthesis of cadmium sulfide (CdS) nanoparticle (NP) cores in the cavity of apoferritin from horse spleen (HsAFr) was performed by a slow chemical reaction synthesis and a two-step synthesis protocol. We found that the CdS NP core synthesis was slow and that premature CdS NP cores were formed in the apoferritin cavity when the concentration of ammonia water was low. It was proven that the control of the ammonia water concentration can govern the CdS NP core synthesis and successfully produce size-controlled CdS NP cores with diameters from 4.7 to 7.1 nm with narrow size dispersion. X-ray powder diffraction (XRD), energy dispersive spectroscopy (EDS) analysis and high-resolution transmission electron microscopy (HR-TEM) observation characterized the CdS NP cores obtained as cubic polycrystalline NPs, which showed photoluminescence with red shifts depending on their diameters. From the research of CdS NP core synthesis in the recombinant apoferritins, the zeta potential of apoferritin is important for the biomineralization of CdS NP cores in the apoferritin cavity. These synthesized CdS NPs with different photoluminescence properties will be applicable in a wide variety of nano-applications.

  18. Ultrasonic-assisted one-pot preparation of ZnO/Ag3VO4 nanocomposites for efficiently degradation of organic pollutants under visible-light irradiation

    NASA Astrophysics Data System (ADS)

    Kiantazh, Fariba; Habibi-Yangjeh, Aziz

    2015-11-01

    We report a facile ultrasonic-assisted one-pot method for preparation of ZnO/Ag3VO4 nanocomposites with different mole fractions of silver vanadate. The preparation method has considerable merits such as short preparation time, large-scale, and one-pot strategy. The resultant samples were fairly characterized by means of XRD, EDX, SEM, TEM, UV-vis DRS, FT-IR, and PL techniques. Visible-light activity of the resultant samples was investigated by degradation of rhodamine B (RhB), methylene blue (MB), and methyl orange (MO). Among the prepared nanocomposites, the ZnO/Ag3VO4 nanocomposite with 0.073 mole fraction of Ag3VO4 exhibited the best activity and excessive amount of Ag3VO4 resulted in decrease of the activity. Photocatalytic activity of this nanocomposite under visible-light irradiation is about 21, 56, and 2.8-fold higher than that of the ZnO sample in degradation of RhB, MB, and MO, respectively. The highly enhanced activity of the nanocomposite was attributed to greater generation of electron-hole pairs, due to photosensitizing role of Ag3VO4 under visible-light irradiation, and efficiently separation of the photogenerated electron-hole pairs, due to formation of n-n heterojunction between the counterparts. Furthermore, it was revealed that the photocatalytic activity largely depends on ultrasonic irradiation time, calcination temperature, and scavengers of the reactive species.

  19. One pot synthesis of diarylfurans from aryl esters and PhI(OAc)2 via palladium-associated iodonium ylides.

    PubMed

    Bao, Yong-Sheng; Agula, Bao; Zhaorigetu, Bao; Jia, Meilin; Baiyin, Menghe

    2015-04-14

    The example of palladium-catalyzed intermolecular cyclization for the synthesis of various diarylfurans in which one of the aromatic rings originates from the phenolic part of the starting ester and the other one from PhI(OAc)2 has been reported. The reaction is carried out through two steps: the rearrangement of palladium-associated iodonium ylides to form o-iodo diaryl ether and then palladium catalyzed intramolecular direct arylation. This reaction can tolerate a variety of functional groups and is alternative or complementary to the previous methods for the synthesis of diarylfurans.

  20. One pot three components microwave assisted and conventional synthesis of new 3-(4-chloro-2-hydroxyphenyl)-2-(substituted) thiazolidin-4-one as antimicrobial agents.

    PubMed

    Pansare, Dattatraya N; Mulla, Nayeem A; Pawar, Chandrakant D; Shende, Vikas R; Shinde, Devanand B

    2014-08-01

    A one-pot, three-component, microwave assisted and conventional synthesis of new 3-(4-chloro-2-hydroxyphenyl)-2-(substituted) thiazolidin-4-one (4a-n) was carried out by using N,N-dimethylformamide as a solvent with high product yield. Among these synthesized compounds (4f, 4g, 4l and 4m) were found to be a broad spectrum molecule active against all bacterial and fungus strains tested, except fungus Aspergillus niger. Amongst the compounds (4g, 4l and 4m) were found to be more potent than respective standard drugs used in the experiment against Candida albicans, Staphylococcus aureus and Aspergillus flavus, respectively. All synthesized compounds were also tested for their cytotoxic activity against HeLa and MCF-7 cell lines by the sulforhodamine B (SRB) assay. This study shows that all compounds were non-cytotoxic in nature, and confirmed their antimicrobial specificity apart from any general cytotoxicity.

  1. Facile one-pot synthesis of L-proline-stabilized fluorescent gold nanoclusters and its application as sensing probes for serum iron.

    PubMed

    Mu, Xiaoyu; Qi, Li; Dong, Ping; Qiao, Juan; Hou, Jian; Nie, Zongxiu; Ma, Huimin

    2013-11-15

    Gold nanoclusters (Au NCs) possess outstanding physical and chemical attributes that make them excellent scaffolds for the construction of novel chemical and biological sensors. In this study, a simple one-pot synthesis method, employing l-proline as the stabilizer, was presented for preparation of fluorescent Au NCs. This strategy allowed the generation of water-soluble Au NCs within a short time of 15 min. The as-prepared Au NCs exhibited a bluish fluorescence emission at 440 nm and a quantum yield of 2.94%. Based on the aggregation-induced fluorescence quenching mechanism, the Au NCs provided favorable biocompatibility, high sensitivity and good selectivity for the measurement of ferric ion (Fe(3+)). Furthermore, serum samples were analyzed for the serum iron contents by using this proposed biocompatible fluorescent sensor, indicating the potential value of this Au NCs-based fluorescent sensor for application in biological and clinical analysis.

  2. A One-Pot Synthesis of m-Terphenyls: A Guided Exploration of Reaction Chemistry, Chromatography, and Spectroscopy. A Miniproject for the Advanced Organic Chemistry Laboratory

    NASA Astrophysics Data System (ADS)

    Anam, Kishorekumar T.; Curtis, Michael P.; Irfan, Muhammad J.; Johnson, Michael P.; Royer, Andrew P.; Shahmohammadi, Kianor; Vinod, Thottumkara K.

    2002-05-01

    This four-week project-based laboratory exercise, developed for advanced organic chemistry students, involves a one-pot synthesis of m-terphenyls. Chemistry of aryl diazonium salts and Grignard reagents and reactivity of aryne intermediates toward nucleophilic reagents form the reaction chemistry basis for the project. The project exposes students to a number of important laboratory techniques (thin-layer chromatography, gas chromatography-mass spectrometry, and column chromatography) for monitoring reaction progress and product isolation. A variety of spectroscopic techniques, including IR, 1H NMR, 13C NMR, and attached proton test are used for product characterization. Students are also introduced to a useful empirical relationship to help predict (with considerable accuracy) the 13C chemical shift values of carbon atoms of substituted benzenes.

  3. Effective one-pot multienzyme (OPME) synthesis of monotreme milk oligosaccharides and other sialosides containing 4-O-acetyl sialic acid.

    PubMed

    Yu, Hai; Zeng, Jie; Li, Yanhong; Thon, Vireak; Shi, Baojun; Chen, Xi

    2016-09-28

    A facile one-pot two-enzyme chemoenzymatic approach has been established for the gram (Neu4,5Ac2α3Lac, 1.33 g) and preparative scale (Neu4,5Ac2α3LNnT) synthesis of monotreme milk oligosaccharides. Other O-acetyl-5-N-acetylneuraminic acid (Neu4,5Ac2)- or 4-O-acetyl-5-N-glycolylneuraminic acid (Neu4Ac5Gc) -containing α2-3-sialosides have also been synthesized in the preparative scale. Used as an effective probe, Neu4,5Ac2α3GalβpNP was found to be a suitable substrate by human influenza A viruses but not bacterial sialidases. PMID:27548611

  4. One-pot three-component synthesis of alpha-iminonitriles by IBX/TBAB-mediated oxidative Strecker reaction.

    PubMed

    Fontaine, Patrice; Chiaroni, Angèle; Masson, Géraldine; Zhu, Jieping

    2008-04-17

    The reaction of aldehydes, amines, and TMSCN in the presence of 2-iodoxybenzoic acid (IBX) and tetrabutylammonium bromide (TBAB) afforded alpha-iminonitriles in good to excellent yields under mild conditions. The presence of TBAB is essential for this transformation. The methodology was applied to a two-step synthesis of indolizidine via a microwave-assisted intramolecular cycloaddition of alpha-iminonitrile.

  5. A new one-pot synthesis of novel hetarylazo-heterocyclic colorants and study of their solvatochromic properties.

    PubMed

    Shawali, Ahmad S; Abdallah, Magda A; Kandil, Mohamed A

    2015-09-01

    A simple synthetic strategy for synthesis of new series of hetarylazo-heterocycles is described. The effects of solvent on their electronic absorption spectra were analyzed using Kamlet-Taft equation. The results of fitting coefficients indicated that the solvatochromism of the studied compounds is mainly due to the solvent polarity rather than the solvent basicity and acidity. PMID:27330835

  6. A new one-pot synthesis of novel hetarylazo-heterocyclic colorants and study of their solvatochromic properties.

    PubMed

    Shawali, Ahmad S; Abdallah, Magda A; Kandil, Mohamed A

    2015-09-01

    A simple synthetic strategy for synthesis of new series of hetarylazo-heterocycles is described. The effects of solvent on their electronic absorption spectra were analyzed using Kamlet-Taft equation. The results of fitting coefficients indicated that the solvatochromism of the studied compounds is mainly due to the solvent polarity rather than the solvent basicity and acidity.

  7. One-pot synthesis and visible light photocatalytic activity of monodispersed AgIn{sub 5}S{sub 8} microspheres

    SciTech Connect

    Li, Xiangqing; Wang, Lei; Wei, Dailong; Kang, Shizhao; Mu, Jin

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► Monodispersed AgIn{sub 5}S{sub 8} microspheres were prepared in a one-pot process. ► The process is environmental friendly. ► The AgIn{sub 5}S{sub 8} microspheres display high photocatalytic activity. -- Abstract: Monodispersed AgIn{sub 5}S{sub 8} microspheres were synthesized using a one-pot solution method and characterized with X-ray diffraction, UV–vis diffuse reflectance spectroscopy, scanning electron microscope, energy dispersive X-ray spectroscopy and N{sub 2} adsorption–desorption isotherm. The results indicated that the AgIn{sub 5}S{sub 8} microspheres were of cubic spinel structure and the mean diameter of about 0.5 μm. In addition, the visible light photocatalytic activity of AgIn{sub 5}S{sub 8} microspheres was also investigated at room temperature. The AgIn{sub 5}S{sub 8} microspheres showed very high photocatalytic activity for the degradation of methyl orange with a degradation efficiency of about 98% under visible light irradiation for 20 min.

  8. One-Pot Synthesis of Fe(III)-Polydopamine Complex Nanospheres: Morphological Evolution, Mechanism, and Application of the Carbonized Hybrid Nanospheres in Catalysis and Zn-Air Battery.

    PubMed

    Ang, Jia Ming; Du, Yonghua; Tay, Boon Ying; Zhao, Chenyang; Kong, Junhua; Stubbs, Ludger Paul; Lu, Xuehong

    2016-09-13

    We report one-pot synthesis of Fe(III)-polydopamine (PDA) complex nanospheres, their structures, morphology evolution, and underlying mechanism. The complex nanospheres were synthesized by introducing ferric ions into the reaction mixture used for polymerization of dopamine. It is verified that both the oxidative polymerization of dopamine and Fe(III)-PDA complexation contribute to the "polymerization" process, in which the ferric ions form coordination bonds with both oxygen and nitrogen, as indicated by X-ray absorption fine-structure spectroscopy. In the "polymerization" process, the morphology of the complex nanostructures is gradually transformed from sheetlike to spherical at the feed Fe(III)/dopamine molar ratio of 1/3. The final size of the complex spheres is much smaller than its neat PDA counterpart. At higher feed Fe(III)/dopamine molar ratios, the final morphology of the "polymerization" products is sheetlike. The results suggest that the formation of spherical morphology is likely to be driven by covalent polymerization-induced decrease of hydrophilic functional groups, which causes reself-assembly of the PDA oligomers to reduce surface area. We also demonstrate that this one-pot synthesis route for hybrid nanospheres enables the facile construction of carbonized PDA (C-PDA) nanospheres uniformly embedded with Fe3O4 nanoparticles of only 3-5 nm in size. The C-PDA/Fe3O4 nanospheres exhibit catalytic activity toward oxygen reduction reaction and deliver a stable discharge voltage for over 200 h when utilized as the cathode in a primary Zn-air battery and are also good recyclable catalyst supports.

  9. One-Pot Synthesis of Fe(III)-Polydopamine Complex Nanospheres: Morphological Evolution, Mechanism, and Application of the Carbonized Hybrid Nanospheres in Catalysis and Zn-Air Battery.

    PubMed

    Ang, Jia Ming; Du, Yonghua; Tay, Boon Ying; Zhao, Chenyang; Kong, Junhua; Stubbs, Ludger Paul; Lu, Xuehong

    2016-09-13

    We report one-pot synthesis of Fe(III)-polydopamine (PDA) complex nanospheres, their structures, morphology evolution, and underlying mechanism. The complex nanospheres were synthesized by introducing ferric ions into the reaction mixture used for polymerization of dopamine. It is verified that both the oxidative polymerization of dopamine and Fe(III)-PDA complexation contribute to the "polymerization" process, in which the ferric ions form coordination bonds with both oxygen and nitrogen, as indicated by X-ray absorption fine-structure spectroscopy. In the "polymerization" process, the morphology of the complex nanostructures is gradually transformed from sheetlike to spherical at the feed Fe(III)/dopamine molar ratio of 1/3. The final size of the complex spheres is much smaller than its neat PDA counterpart. At higher feed Fe(III)/dopamine molar ratios, the final morphology of the "polymerization" products is sheetlike. The results suggest that the formation of spherical morphology is likely to be driven by covalent polymerization-induced decrease of hydrophilic functional groups, which causes reself-assembly of the PDA oligomers to reduce surface area. We also demonstrate that this one-pot synthesis route for hybrid nanospheres enables the facile construction of carbonized PDA (C-PDA) nanospheres uniformly embedded with Fe3O4 nanoparticles of only 3-5 nm in size. The C-PDA/Fe3O4 nanospheres exhibit catalytic activity toward oxygen reduction reaction and deliver a stable discharge voltage for over 200 h when utilized as the cathode in a primary Zn-air battery and are also good recyclable catalyst supports. PMID:27550631

  10. One-pot synthesis of size- and morphology-controlled 1-D iron oxide nanochains with manipulated magnetic properties.

    PubMed

    He, Qingliang; Yuan, Tingting; Yan, Xingru; Luo, Zhiping; Haldolaarachchige, Neel; Young, David P; Wei, Suying; Guo, Zhanhu

    2014-01-01

    Polypropylene grafted maleic anhydride (PP-MA, 2500 g mole(-1)) has demonstrated its unique capability to synthesize 1-D ferromagnetic hard (292.7 Oe) γ-Fe2O3 nanochains made of ~24 nm nanoparticles vs. PP-MA with 8000 g mole(-1) for the synthesis of 1-D ferromagnetic soft (70.5 Oe) γ-Fe2O3 nanochains (30 nm) made of flowerlike nanoparticles.

  11. Skeletally Diverse Synthesis of Indole-Fused Diazocine and Diazepine Frameworks by One-Pot, Two-Component Cascade Reaction.

    PubMed

    Thikekar, Tushar Ulhas; Selvaraju, Manikandan; Sun, Chung-Ming

    2016-01-15

    An expeditious and novel strategy has been explored for the synthesis of structurally diverse indole-fused diazocine and diazepine derivatives. A substrate-based diversification approach of methyl-3-aminoindole/indoline benzoates coupled with the Pictet-Spengler reaction and three different reaction cascades furnished indolodiazepine and indoloquinoxalines. The formation of indolodiazocines proceeds through an initial condensation followed by intramolecular alkylation. PMID:26735127

  12. An efficient one pot syntheses of aryl-3,3'-bis(indolyl)methanes and studies on their spectral characteristics, DPPH radical scavenging-, antimicrobial-, cytotoxicity-, and antituberculosis activity

    NASA Astrophysics Data System (ADS)

    Suresh Kumar, G. S.; Kumaresan, S.; Antony Muthu Prabhu, A.; Bhuvanesh, N.; Seethalakshmi, P. G.

    2013-01-01

    An efficient one-pot syntheses of aryl-3,3'-bis(indolyl)methanes (BIMs) from indole/2-methylindole and formylphenoxyaliphatic acid(s) is described. Esterification of carboxylic acid and aromatic electrophilic substitution reactions are achieved simultaneous in the presence of potash alum as a catalyst. This catalyst could be recovered and reused without substantial loss in its catalytic activity and the methodology could be applied on a range of closely related substrates. The solvation characteristics in ground and excited states of the compounds by monitoring the absorbance and fluorescence band maxima have been studied. The fluorescence studies in protic and aprotic solvents were rationalized on the basis of solute-solvent interaction and substituents effect on these photophysical processes analyzed. The compounds prepared showed efficient antimicrobial effect against human pathogens, cytotoxicity against A431 cell line, and DPPH radical scavenging effect. Single crystal XRD studies have been carried out for a few compounds synthesized in this work.

  13. One-pot synthesis of functionalized 2,5-dihydrofurans via an amine-promoted Petasis borono-Mannich reaction.

    PubMed

    Cui, Chun-Xiao; Li, Hui; Yang, Xian-Jin; Yang, Jun; Li, Xiao-Qiang

    2013-12-01

    A series of functionalized 2,5-dihydrofurans were efficiently synthesized via an amine-promoted Petasis borono-Mannich reaction of 4-substituted 1,2-oxaborol-2(5H)-ols with salicylaldehydes in high yields. The process, which combines a boronic acid-based Mannich reaction and a highly efficient intramolecular SN2 cyclization, provides a one-step and efficient route toward 2,5-dihydrofurans from simple and stable starting materials.

  14. Petasis Borono-Mannich reaction and allylation of carbonyl compounds via transient allyl boronates generated by palladium-catalyzed substitution of allyl alcohols. an efficient one-pot route to stereodefined alpha-amino acids and homoallyl alcohols.

    PubMed

    Selander, Nicklas; Kipke, Andreas; Sebelius, Sara; Szabó, Kalman J

    2007-11-01

    An efficient one-pot procedure was designed by integration of the pincer-complex-catalyzed borylation of allyl alcohols in the Petasis borono-Mannich reaction and in allylation of aldehydes and ketones. These procedures are suitable for one-pot synthesis of alpha-amino acids and homoallyl alcohols from easily available allyl alcohol, amine, aldehyde, or ketone substrates. In the presented transformations, the active allylating agents are in situ generated allyl boronic acid derivatives. These transient intermediates are proved to be reasonably acid-, base-, alcohol-, water-, and air-stable species, which allows a high level of compatibility with the reaction conditions of the allylation of various aldehyde/ketone and imine electrophiles. The boronate source of the reaction is diboronic acid or in situ hydrolyzed diboronate ester ensuring that the waste product of the reaction is nontoxic boric acid. The regio- and stereoselectivity of the reaction is excellent, as almost all products form as single regio- and stereoisomers. The described procedure is suitable to create quaternary carbon centers in branched allylic products without formation of the corresponding linear allylic isomers. Furthermore, products comprising three stereocenters were formed as single products without formation of other diastereomers. Because of the highly disciplined consecutive processes, up to four-step, four-component transformations could be performed selectively as a one-pot sequence. For example, stereodefined pyroglutamic acid could be prepared from a simple allyl alcohol, a commercially available amine, and glyoxylic acid in a one-step procedure. The presented method also grants an easy access to stereodefined 1,7-dienes that are useful substrates for Grubbs ring-closing metathesis.

  15. Biomimetic one-pot synthesis of gold nanoclusters/nanoparticles for targeted tumor cellular dual-modality imaging

    NASA Astrophysics Data System (ADS)

    Lin, Jing; Zhou, Zhijun; Li, Zhiming; Zhang, Chunlei; Wang, Xiansong; Wang, Kan; Gao, Guo; Huang, Peng; Cui, Daxiang

    2013-04-01

    Biomimetic synthesis has become a promising green pathway to prepare nanomaterials. In this study, bovine serum albumin (BSA)-conjugated gold nanoclusters/nanoparticles were successfully synthesized in water at room temperature by a protein-directed, solution-phase, green synthetic method. The synthesized BSA-Au nanocomplexes have fluorescence emission (588 nm) of gold nanoclusters and surface plasmon resonance of gold nanoparticles. The BSA-Au nanocomplexes display non-cytotoxicity and excellent biocompatibility on MGC803 gastric cancer cells. After conjugation of folic acid molecules, the obtained BSA-Au nanocomplexes showed highly selective targeting for MGC803 cells and dual-modality dark-field and fluorescence imaging.

  16. Cu(II) /TEMPO-promoted one-pot synthesis of highly substituted pyrimidines from amino acid esters.

    PubMed

    Zhou, Nini; Xie, Tao; Li, Zhongle; Xie, Zhixiang

    2014-12-22

    A novel, Cu(OAc)2/TEMPO promoted one-step approach for the preparation of fully substituted pyrimidines from readily available amino acid esters has been described. In this reaction, the amino acid esters act as the only N-C sources for the construction of corresponding pyrimidines. The mechanism of this process includes oxidative dehydrogenation, the generation of an imine radical, and a formal [3+3] cycloaddition. This methodology proves to be a high atom-economic and straightforward strategy for the synthesis of pyrimidines and diverse substrates which are substituted by various functional groups have been afforded in moderate to good yield. PMID:25377658

  17. One-pot synthesis of cuprous oxide-reduced graphene oxide nanocomposite with enhanced photocatalytic and electrocatalytic performance

    NASA Astrophysics Data System (ADS)

    Han, Fugui; Li, Heping; Yang, Jun; Cai, Xiaodong; Fu, Li

    2016-03-01

    We report on the facile one-step synthesis of porous cuprous oxide nanoparticles on reduced graphene oxide (Cu2O-RGO) by synchronously reducing Cu2+ ions and GO with ethylene glycol. The basic chemical components, crystal structure and surface morphology of prepared nanocomposite was carefully characterized. The photocatalytic activities of the as-prepared nanocomposite was investigated by photodegrading methylene blue (MB) under visible light. The electrocatalytic property of the nanocomposite was investigated by electrocatalytic determination of acetaminophen. The results indicate that the corporation of RGO with Cu2O nanoparticles could high enhance the both photocatalytic and electrocatalytic properties. Moreover, we found that the content of RGO introduced into nanocomposite could highly affect the product properties.

  18. Biomimetic one-pot synthesis of gold nanoclusters/nanoparticles for targeted tumor cellular dual-modality imaging

    PubMed Central

    2013-01-01

    Biomimetic synthesis has become a promising green pathway to prepare nanomaterials. In this study, bovine serum albumin (BSA)-conjugated gold nanoclusters/nanoparticles were successfully synthesized in water at room temperature by a protein-directed, solution-phase, green synthetic method. The synthesized BSA-Au nanocomplexes have fluorescence emission (588 nm) of gold nanoclusters and surface plasmon resonance of gold nanoparticles. The BSA-Au nanocomplexes display non-cytotoxicity and excellent biocompatibility on MGC803 gastric cancer cells. After conjugation of folic acid molecules, the obtained BSA-Au nanocomplexes showed highly selective targeting for MGC803 cells and dual-modality dark-field and fluorescence imaging. PMID:23587362

  19. One-Pot Synthesis and Evaluation of Antileishmanial Activities of Functionalized S-Alkyl/Aryl Benzothiazole-2-carbothioate Scaffold.

    PubMed

    Dar, Ajaz A; Shadab, M; Khan, Suman; Ali, Nahid; Khan, Abu T

    2016-04-15

    The synthesis of hitherto unreported S-alkyl/aryl benzothiazole-2-carbothioate is reported from thiols, oxalyl chloride, and 2-aminothiophenols using 10 mol % n-tetrabutylammonium iodide (TBAI) as catalyst in acetonitrile through multicomponent reaction (MCR) strategy. The present protocol favored formation of benzothiazoles and thioesters via simultaneous formation of C-N and C-S bonds in good yields with a wide range of substrates. A few of the synthesized derivatives were evaluated for their antimicrobial activity against the protozoan parasite Leishmania donovani, a causative agent of visceral leishmaniasis (VL). Further, these compounds displayed no toxicity toward macrophage RAW 264.7 cells and are therefore nontoxic and effective antileishmanial leads. In silico docking studies were performed to understand the possible binding site interaction with trypanothione reductase (TryR).

  20. Statistical Experimental Design Guided Optimization of a One-Pot Biphasic Multienzyme Total Synthesis of Amorpha-4,11-diene

    PubMed Central

    Chen, Xixian; Zhang, Congqiang; Zou, Ruiyang; Zhou, Kang; Stephanopoulos, Gregory; Too, Heng Phon

    2013-01-01

    In vitro synthesis of chemicals and pharmaceuticals using enzymes is of considerable interest as these biocatalysts facilitate a wide variety of reactions under mild conditions with excellent regio-, chemo- and stereoselectivities. A significant challenge in a multi-enzymatic reaction is the need to optimize the various steps involved simultaneously so as to obtain high-yield of a product. In this study, statistical experimental design was used to guide the optimization of a total synthesis of amorpha-4,11-diene (AD) using multienzymes in the mevalonate pathway. A combinatorial approach guided by Taguchi orthogonal array design identified the local optimum enzymatic activity ratio for Erg12:Erg8:Erg19:Idi:IspA to be 100∶100∶1∶25∶5, with a constant concentration of amorpha-4,11-diene synthase (Ads, 100 mg/L). The model also identified an unexpected inhibitory effect of farnesyl pyrophosphate synthase (IspA), where the activity was negatively correlated with AD yield. This was due to the precipitation of farnesyl pyrophosphate (FPP), the product of IspA. Response surface methodology was then used to optimize IspA and Ads activities simultaneously so as to minimize the accumulation of FPP and the result showed that Ads to be a critical factor. By increasing the concentration of Ads, a complete conversion (∼100%) of mevalonic acid (MVA) to AD was achieved. Monovalent ions and pH were effective means of enhancing the specific Ads activity and specific AD yield significantly. The results from this study represent the first in vitro reconstitution of the mevalonate pathway for the production of an isoprenoid and the approaches developed herein may be used to produce other isopentenyl pyrophosphate (IPP)/dimethylallyl pyrophosphate (DMAPP) based products. PMID:24278153

  1. A Novel and Facile One-Pot Solvothermal Synthesis of PEDOT-PSS/Ni-Mn-Co-O Hybrid as an Advanced Supercapacitor Electrode Material.

    PubMed

    Yin, Chengjie; Yang, Chunming; Jiang, Min; Deng, Cuifen; Yang, Lishan; Li, Junhua; Qian, Dong

    2016-02-01

    In this work, a novel and facile one-pot method has been developed for the synthesis of a hybrid consisting of Ni-Mn-Co ternary oxide and poly(3,4-ethylenedioxythiophene)-polystyrenesulfonate (PEDOT-PSS/NMCO) with a hierarchical three-dimensional net structure via a solvothermal-coprecipitation coupled with oxidative polymerization route. Apart from the achievement of polymerization, coprecipitation, and solvothermal in one pot, the hydroxyl (OH(-)) ions generated from the oxidative polymerization of organic monomer by neutral KMnO4 solution were skillfully employed as precipitants for metal ions. As compared with the PEDOT-PSS/Ni-Mn binary oxide, PEDOT-PSS/Co-Mn binary oxide, and PEDOT-PSS/MnO2, PEDOT-PSS1.5/NMCO exhibits overwhelmingly superior supercapacitive performance, more specifically, a high specific capacitance of 1234.5 F g(-1) at a current density of 1 A g(-1), a good capacitance retention of 83.7% at a high current density of 5 A g(-1) after 1000 cycles, an energy density of 51.9 W h kg(-1) at a power density of 275 W kg(-1), and an energy density of 21.4 W h kg(-1) at an extremely elevated power density of 5500 W kg(-1). Noticeably, the energy density and power density of PEDOT-PSS/NMCO are by far higher than those of the existing analogues recently reported. The exceptional performance of PEDOT-PSS/NMCO benefits from its unique mesoporous architecture, which could provide a larger reaction surface area, faster ion and electron transfer ability, and good structural stability. The desirable integrated performance enables the multicomponent composite to be a promising electrode material for energy storage applications. PMID:26794146

  2. One-pot three-component synthesis of novel heterocyclic steroids as a central antioxidant and anti-inflammatory agents.

    PubMed

    Mohamed, Nadia R; Abdelhalim, Mervat M; Khadrawy, Yasser A; Elmegeed, Gamal A; Abdel-Salam, Omar M E

    2012-11-01

    Oxidative stress and inflammation have been implicated in several neurodegenerative and developmental brain disorders. The present work was devoted to the design and synthesis of novel steroid derivatives bearing promising heterocyclic moiety that would act to reduce neuro-inflammation and oxidative stress in brain. The novel heterocyclic steroids were synthesized and their chemical structures were confirmed by studying their analytical and spectral data. The tested compounds were assayed in the model of neuro-inflammation produced in rats by cerebral lipopolysaccharide injection. The intracerebral administration of bacterial endotoxin resulted in cerebral inflammatory state evidenced by increased malondialdehyde (MDA), decreased reduced glutathione (GSH) level, increased nitric oxide as well as increased acetylcholinesterase (AChE) activity in the brain. Compounds 6, 10, 8b and 13a markedly increased reduced glutathione. Malondialadehyde and nitric oxide levels were reduced to normal values after treatment with all tested compounds. AChE activity was normalized by compound 8b and reduced to below normal values by compounds 10 and 14a. These results are exciting in that these agents might be useful candidates in treatment of cerebral inflammation.

  3. One-pot synthesis of magnetic graphene nanocomposites decorated with core@double-shell nanoparticles for fast chromium removal.

    PubMed

    Zhu, Jiahua; Wei, Suying; Gu, Hongbo; Rapole, Sowjanya B; Wang, Qiang; Luo, Zhiping; Haldolaarachchige, Neel; Young, David P; Guo, Zhanhu

    2012-01-17

    A facile thermodecomposition process to synthesize magnetic graphene nanocomposites (MGNCs) is reported. High-resolution transmission electron microscopy and energy filtered elemental mapping revealed a core@double-shell structure of the nanoparticles with crystalline iron as the core, iron oxide as the inner shell and amorphous Si-S-O compound as the outer shell. The MGNCs demonstrate an extremely fast Cr(VI) removal from the wastewater with a high removal efficiency and with an almost complete removal of Cr(VI) within 5 min. The adsorption kinetics follows the pseudo-second-order model and the novel MGNC adsorbent exhibits better Cr(VI) removal efficiency in solutions with low pH. The large saturation magnetization (96.3 emu/g) of the synthesized nanoparticles allows fast separation of the MGNCs from liquid suspension. By using a permanent magnet, the recycling process of both the MGNC adsorbents and the adsorbed Cr(VI) is more energetically and economically sustainable. The significantly reduced treatment time required to remove the Cr(VI) and the applicability in treating the solutions with low pH make MGNCs promising for the efficient removal of heavy metals from the wastewater. PMID:22126606

  4. One-pot synthesis of magnetic Ni@Mg(OH)2 core-shell nanocomposites as a recyclable removal agent for heavy metals.

    PubMed

    Zhang, Meng; Song, Weiqiang; Chen, Qiuling; Miao, Baoji; He, Weichun

    2015-01-28

    A surfactant-assisted hydrothermal route has been presented to one-pot synthesized Ni nanoparticles encapsulated in Mg(OH)2 hollow spheres. The diameter of Ni cores and the thickness of Mg(OH)2 shells are about 60-80 and 15 nm, respectively, and the size of a whole composite sphere is approximately 70-100 nm. Benefiting from the ferrimagnetic behavior of Ni cores and the high surface area of Mg(OH)2 shells, Ni@Mg(OH)2 nanocomposites exhibit excellent heavy metals adsorption capacity and recyclable property. The first removal efficiency is almost 100% for target metals, and after five cycles, the adsorption capacity remains 95%. A series of experiments show the adsorption of heavy metal ions on Ni@Mg(OH)2 follows a pseudo-second order kinetic equation and can be described by a Langmuir isotherm model.

  5. Facile one pot synthesis of zinc oxide nanorods and statistical evaluation for photocatalytic degradation of a diazo dye.

    PubMed

    Dutta, Suvanka; Ghosh, Ananya; Kabir, Humayun; Saha, Rajnarayan

    2016-01-01

    In the present work zinc oxide nanorods (ZNRs) have been synthesized to estimate its photocatalytic degradation potential on an industrially used diazo dye and optimization of the total treatment process has been designed. Response surface methodology (RSM) has been used to model the operational parameters for this photocatalytic degradation. The crystallite size (101 plane) of the synthesized ZNR has been found to be 20.99 nm having a band gap energy of 3.45 eV. At elevated pH, the rate of degradation of the photocatalyst was found to be higher than that of acidic pH. The independent variables of the model are time (9.6-122 min), pH (2-12.2), catalyst dose (0.2-0.4 g/L) and dye concentration (88-512 mg/L). It was seen that the degradation efficiency was significantly affected by the initial dye concentration and the pH, the optimal values of the parameters being a pH of 10.67, an initial concentration of 150 mg/L and ZnO dose of 0.37 g/L, the time taken being 88.52 min. The actual degradation efficiency of the dye reached 96.9% at optimized condition, which is quite close to the predicted value of 98.07%. PMID:27508375

  6. One-pot synthesis of crosslinked amphiphilic polycarbonates as stable but reduction-sensitive carriers for doxorubicin delivery

    NASA Astrophysics Data System (ADS)

    Yi, Xiaoqing; Zhang, Quan; Dong, Hui; Zhao, Dan; Xu, Jia-qi; Zhuo, Renxi; Li, Feng

    2015-10-01

    In this paper, we first synthesized a novel disulfide-coupled bis-(cyclic carbonate) (TDCSS) monomer. After ring-opening co-polymerization (ROP) of TDCSS and trimethylene carbonate (TMC) initiated by mono-methoxyl poly(ethylene glycol), the crosslinked reduction-sensitive copolymer PEG-P(TMC-co-TDCSS) was obtained via a facile one-step procedure for efficient delivery of doxorubicin (DOX) into cancer cells. To serve as controls, PEG-P(TMC-co-TDCCC), which has an analogous structure without disulfide bond, and a linear polymer PEG-PTMC were also prepared. The copolymers could self-assemble to form nano-sized micelles in an aqueous solution. As compared to PEG-PTMC, crosslinked PEG-P(TMC-co-TDCSS) and PEG-P(TMC-co-TDCCC) showed lower CMC values and thus induced a much better micelle-forming ability. In vitro release studies revealed that the drug release behavior of DOX-loaded PEG-P(TMC-co-TDCSS) micelles, which could be accelerated in the presence of 10 mM dithiothreitol (DTT), showed a similar trend in the absence of DTT compared to DOX-loaded PEG-P(TMC-co-TDCCC) micelles. Furthermore, confocal laser scanning microscopy (CLSM) indicated that DOX-loaded PEG-P(TMC-co-TDCSS) micelles were efficiently internalized into HeLa cells, releasing DOX into the cytoplasm after which the drug finally entered the nuclei, while MTT assays also demonstrated potent cytotoxic activity against HeLa cells. DOX was mainly located in the cytoplasm for reduction-insensitive PEG-P(TMC-co-TDCCC) and PEG-PTMC controls.

  7. One-pot synthesis of crosslinked amphiphilic polycarbonates as stable but reduction-sensitive carriers for doxorubicin delivery.

    PubMed

    Yi, Xiaoqing; Zhang, Quan; Dong, Hui; Zhao, Dan; Xu, Jia-qi; Zhuo, Renxi; Li, Feng

    2015-10-01

    In this paper, we first synthesized a novel disulfide-coupled bis-(cyclic carbonate) (TDCSS) monomer. After ring-opening co-polymerization (ROP) of TDCSS and trimethylene carbonate (TMC) initiated by mono-methoxyl poly(ethylene glycol), the crosslinked reduction-sensitive copolymer PEG-P(TMC-co-TDCSS) was obtained via a facile one-step procedure for efficient delivery of doxorubicin (DOX) into cancer cells. To serve as controls, PEG-P(TMC-co-TDCCC), which has an analogous structure without disulfide bond, and a linear polymer PEG-PTMC were also prepared. The copolymers could self-assemble to form nano-sized micelles in an aqueous solution. As compared to PEG-PTMC, crosslinked PEG-P(TMC-co-TDCSS) and PEG-P(TMC-co-TDCCC) showed lower CMC values and thus induced a much better micelle-forming ability. In vitro release studies revealed that the drug release behavior of DOX-loaded PEG-P(TMC-co-TDCSS) micelles, which could be accelerated in the presence of 10 mM dithiothreitol (DTT), showed a similar trend in the absence of DTT compared to DOX-loaded PEG-P(TMC-co-TDCCC) micelles. Furthermore, confocal laser scanning microscopy (CLSM) indicated that DOX-loaded PEG-P(TMC-co-TDCSS) micelles were efficiently internalized into HeLa cells, releasing DOX into the cytoplasm after which the drug finally entered the nuclei, while MTT assays also demonstrated potent cytotoxic activity against HeLa cells. DOX was mainly located in the cytoplasm for reduction-insensitive PEG-P(TMC-co-TDCCC) and PEG-PTMC controls. PMID:26357961

  8. Highly efficient one-pot labeling of new phosphonium cations with fluorine-18 as potential PET agents for myocardial perfusion imaging.

    PubMed

    Zhao, Zuoquan; Yu, Qian; Mou, Tiantian; Liu, Chang; Yang, Wenjiang; Fang, Wei; Peng, Cheng; Lu, Jie; Liu, Yu; Zhang, Xianzhong

    2014-11-01

    Lipophilic cations such as phosphonium salts can accumulate in mitochondria of heart in response to the negative inner-transmembrane potentials. Two phosphonium salts [(18)F]FMBTP and [(18)F]mFMBTP were prepared and evaluated as potential myocardial perfusion imaging (MPI) agents in this study. The cations were radiolabeled via a simplified one-pot method starting from [(18)F]fluoride and followed by physicochemical property tests, in vitro cellular uptake assay, ex vivo mouse biodistribution, and in vivo rat microPET imaging. The total radiosynthesis time was less than 60 min including HPLC purification. The [(18)F] labeled compounds were obtained in high radiolabeling yield (∼50%) and good radiochemical purity (>99%). Both compounds were electropositive, and their log P values at pH 7.4 were 1.16 ± 0.003 (n = 3) and 1.05 ± 0.01 (n = 3), respectively. Both [(18)F]FMBTP and [(18)F]mFMBTP had high heart uptake (25.24 ± 2.97% ID/g and 31.02 ± 0.33% ID/g at 5 min postinjection (p.i.)) in mice with good retention (28.99 ± 3.54% ID/g and 26.82 ± 3.46% ID/g at 120 min p.i.). From the PET images in rats, the cations exhibited high myocardium uptake and fast clearance from liver and small intestine to give high-contrast images across all time points. These phosphonium cations were radiosynthesized via a highly efficient one-pot procedure for potential MPI offering high heart accumulation and rapid nontarget clearance.

  9. Rapid 'one-pot' synthesis of a novel benzimidazole-5-carboxylate and its hydrazone derivatives as potential anti-inflammatory and antimicrobial agents.

    PubMed

    Vasantha, Kumar; Basavarajaswamy, Guru; Vaishali Rai, M; Boja, Poojary; Pai, Vinitha R; Shruthi, N; Bhat, Mahima

    2015-04-01

    A novel series of N-arylidene-2-(2,4-dichloro phenyl)-1-propyl-1H-benzo[d] imidazole-5-carbohydrazides having different substitution on the arylidene part were synthesized in good yield. The core nucleus benzimidazole-5-carboxylate (5) was efficiently synthesized by 'one-pot' nitro reductive cyclization reaction between ethyl-3-nitro-4-(propylamino)benzoate and 2,4-dichlorobenzaldehyde using sodium dithionite in dimethylsulfoxide. This 'one-pot' reaction was proceeded very smoothly, in short reaction time with an excellent yield. All the compounds (7a-r) were screened for their in vivo anti-inflammatory and in vitro antimicrobial activity. Most of the compounds exhibited remarkable paw-edema inhibition in the initial one hour of administration indicating the higher potentiality of these molecules. In particular, compounds 7a, 7d, 7f and 7g displayed a high level of carrageenan-induced paw edema inhibition compared to that of indomethacin. Compound 7p exhibited very good antibacterial activity and antifungal activity with a MIC of 3.12 μg/mL against most of the tested organisms. Furthermore, compounds 7d, 7f, 7h and 7p found to be good inhibitors of Aspergillus niger with MIC of 3.12 μg/mL. Cytotoxicity of the potent compounds 7d, 7f and 7p was checked using MDA MB-231 breast cancer cell line and are found to be non toxic at the highest concentration used (i.e., 10 μg/mL).

  10. One-pot synthesis of gold nanoclusters with bright red fluorescence and good biorecognition abilities for visualization fluorescence enhancement detection of E. coli.

    PubMed

    Liu, Jiali; Lu, Lili; Xu, Suying; Wang, Leyu

    2015-03-01

    A facile one-pot strategy was developed for the synthesis of lysozyme functionalized fluorescence gold nanoclusters (AuNCs). The lysozymes added to reduce Au(3+) ions and stabilize the AuNCs during the synthesis were coated on the AuNCs surface and retained their specific recognition ability for bacteria such as Escherichia coli (E. coli). Based on such ability, these AuNCs were specifically attached onto the surface of E. coli, which resulted in great red fluorescence enhancement. Nevertheless, the bovine serum albumin (BSA) stabilized AuNCs could not recognize E. coli and no fluorescence enhancement was observed. Upon the addition of E. coli, the red fluorescence intensity of lysozyme-AuNCs was enhanced linearly over the range of 2.4×10(4) -6.0×10(6) CFU/mL of E. coli with high sensitivity (LOD=2.0×10(4) CFU/mL, S/N=3). The visualization fluorescence evolution may enable the rapid and real-time detection of bacteria. This study may be extended to other functional proteins such as antibody, enzyme, and peptide functionalized nanoclusters while retaining the bioactivity of coating proteins and find wide applications in the fields of biochemistry and biomedicine.

  11. Iridium ultrasmall nanoparticles, worm-like chain nanowires, and porous nanodendrites: One-pot solvothermal synthesis and catalytic CO oxidation activity

    NASA Astrophysics Data System (ADS)

    Zhang, Tao; Li, Shuai-Chen; Zhu, Wei; Ke, Jun; Yu, Jing-Wen; Zhang, Zhi-Ping; Dai, Lin-Xiu; Gu, Jun; Zhang, Ya-Wen

    2016-06-01

    We report a facile one-pot solvothermal synthesis of monodisperse iridium (Ir) ultrasmall (1.5-2.5 nm in diameter) nanoparticles (NPs), worm-like chain nanowires (NWs), and porous nanodendrites (NDs), for which CO oxidation reaction has been employed as a probe reaction to investigate the effects of nanoparticle size and surface-capping organics on the catalytic activities. Time-dependent experiments revealed that an oriented attachment mechanism induced by the strong adsorption of halide anions (Br- and I-) on specific facet of Ir nanoclusters or by decreasing the reduction rate of Ir precursors with changing their concentrations during the synthesis was responsible for the formation of Ir NWs and NDs. Annealing tests indicated that an O2-H2 atmosphere treatment turned out to be an effective measure to clean up the surface-capping organics of Ir NPs supported on commercial SiO2. Catalytic CO oxidation reaction illustrated that a significant improvement in the catalytic activity of CO oxidation reaction was achieved together with the changing of activation energies after such atmosphere treatment for the supported catalysts of the ultrasmall Ir NPs. It is noteworthy that this enhancement in catalytic activity could be ascribed to the changes in the surface status (including populations of Ir species in metallic and oxidized states, removal of surface capping organics, the variety of active sites, and total effective active site number) for the supported nanocatalysts during the atmosphere treatment.

  12. One-Pot Synthesis of Monodisperse Noble Metal @ Resorcinol-Formaldehyde (M@RF) and M@Carbon Core-Shell Nanostructure and Their Catalytic Applications.

    PubMed

    Yang, Peipei; Xu, Yong; Chen, Lei; Wang, Xuchun; Zhang, Qiao

    2015-10-27

    We demonstrate that noble metal @ RF core-shell nanostructures can be obtained through a facile one-pot synthesis approach in the absence of any additional surfactants. Monodisperse metal@RF core-shell nanostructures can be produced within 1 h on a large scale. Both the core size and shell thickness can be readily tuned by altering the reaction parameters. Systematic studies reveal that resorcinol could have several functions: it could act as a reactant to form RF resin, and it also could passivate the surface of metallic nanoparticles to prevent them from aggregating. Additionally, for the first time, our results suggest that resorcinol may act as a reducing agent that can reduce metal salts to form metal nanoparticles. The core-shell nanoparticles can be carbonized into M@carbon nanostructures, which have shown great performance in the catalytic hydrogenation of chlorobenzene. This work not only will help to achieve the controllable synthesis of noble metal@RF resin and M@carbon core-shell nanostructures but also will promote research into other RF-based nanostructures and their catalytic applications.

  13. Reduced graphene oxide-Hemin-Au nanohybrids: Facile one-pot synthesis and enhanced electrocatalytic activity towards the reduction of hydrogen peroxide.

    PubMed

    Gu, Chang-Jie; Kong, Fen-Ying; Chen, Zhi-Dong; Fan, Da-He; Fang, Hai-Lin; Wang, Wei

    2016-04-15

    A facile and effective strategy is demonstrated for the synthesis of ternary reduced graphene oxide-Hemin-Au (rGO-H-Au) nanohybrids. The nanohybrids were synthesized through a one-pot in situ reduction of GO and HAuCl4 under alkaline conditions using GO, Hemin and HAuCl4 as the starting materials. The synthesis process can be finished within 1h in a solution phase, without adding any additional surfactant, stabilizing agent and toxic or harsh chemical reducing agents. The resulting nanohybrids were characterized by UV-vis spectroscopy, Raman spectroscopy, transmission electron microscopy (TEM), and so on. Electrochemical measurements showed that the rGO-H-Au nanohybrids exhibited good electrocatalytic activity for the reduction of hydrogen peroxide (H2O2). Based on this property, a simple and highly sensitive amperometric biosensor for H2O2 had been developed. The linear relationships were obtained from 0.1 µM to 40 µM and the detection limit was estimated to be 30 nM. The simple and sensitive sensing platform showed great promising applications in the pharmaceutical, clinical and industrial detection of H2O2.

  14. One-pot synthesis of N-F-Cr-doped anatase TiO2 microspheres with nearly all-(001) surface for enhanced solar absorption

    NASA Astrophysics Data System (ADS)

    Wu, Jin-Ming; Tang, Mei-Lan

    2011-09-01

    The synthesis and clarifications in structure-property relationship for anatase TiO2 crystals exposing (001) facets have attracted much attention. In this paper, a novel titania microsphere with nearly all-(001) surface was synthesized by hydrothermal treatment of a thermal sprayed TiN/Ti coating with HF aqueous solution containing chromium powders. Unlike the conventional (001)-facet exposed anatase crystals, which are highly truncated bipyramids, the crystal achieved in the current investigation is drum-like with a round cross section. The formation of the drum-like crystals was contributed to a balance between the erosion and precipitation of anatase single crystallites. The Cr-doping in anatase was believed to increase the surface deficiency which enhanced the erosion procedure, leading to the drum-like crystals. The XPS analysis confirmed the incorporations of N, F and Cr in the microsized anatase crystals through the one-pot reaction, which led to a significantly enhanced solar absorption. The UV-Vis diffuse reflectance revealed a band-to-band red-shift of the band gap of the anatase crystals to 1.60 eV, which is contributed mainly to the homogeneous Cr-doping.The synthesis and clarifications in structure-property relationship for anatase TiO2 crystals exposing (001) facets have attracted much attention. In this paper, a novel titania microsphere with nearly all-(001) surface was synthesized by hydrothermal treatment of a thermal sprayed TiN/Ti coating with HF aqueous solution containing chromium powders. Unlike the conventional (001)-facet exposed anatase crystals, which are highly truncated bipyramids, the crystal achieved in the current investigation is drum-like with a round cross section. The formation of the drum-like crystals was contributed to a balance between the erosion and precipitation of anatase single crystallites. The Cr-doping in anatase was believed to increase the surface deficiency which enhanced the erosion procedure, leading to the drum

  15. Ceria-Vanadia/Silica-Catalyzed Cascade for C-C and C-O Bond Activation: Green One-Pot Synthesis of 2-Amino-3-cyano-4H-pyrans.

    PubMed

    Maddila, Surya Narayana; Maddila, Suresh; van Zyl, Werner E; Jonnalagadda, Sreekantha B

    2016-02-01

    We designed a ceria-vanadia/silica (Ce-V/SiO2) heterogeneous catalyst and used it for the green and efficient synthesis of 2-amino-3-cyano-4H-pyran derivatives. The green reaction was a multicomponent one-pot condensation of 5,5-dimethylcyclohexane-1,3-dione, aromatic aldehyde, and malononitrile in an eco-compatible solvent (ethanol). The catalyst was synthesized and fully characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area analysis. The reported procedure offers a number of advantages including decreased reaction times, mild conditions, high yields, operational simplicity, and environmentally benign and simple work-up procedures. Furthermore, the catalyst is economical, fully recyclable, and reusable for over five runs while preserving its high activity. The synthesized 2-amino-3-cyano-4H-pyran products can later be used for pharmaceutical purposes. PMID:27308209

  16. Ceria-Vanadia/Silica-Catalyzed Cascade for C-C and C-O Bond Activation: Green One-Pot Synthesis of 2-Amino-3-cyano-4H-pyrans.

    PubMed

    Maddila, Surya Narayana; Maddila, Suresh; van Zyl, Werner E; Jonnalagadda, Sreekantha B

    2016-02-01

    We designed a ceria-vanadia/silica (Ce-V/SiO2) heterogeneous catalyst and used it for the green and efficient synthesis of 2-amino-3-cyano-4H-pyran derivatives. The green reaction was a multicomponent one-pot condensation of 5,5-dimethylcyclohexane-1,3-dione, aromatic aldehyde, and malononitrile in an eco-compatible solvent (ethanol). The catalyst was synthesized and fully characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area analysis. The reported procedure offers a number of advantages including decreased reaction times, mild conditions, high yields, operational simplicity, and environmentally benign and simple work-up procedures. Furthermore, the catalyst is economical, fully recyclable, and reusable for over five runs while preserving its high activity. The synthesized 2-amino-3-cyano-4H-pyran products can later be used for pharmaceutical purposes.

  17. Three-component, one-pot synthesis of benzo[6,7]cyclohepta[1,2-b]pyridine derivatives under catalyst free conditions and evaluation of their anti-inflammatory activity.

    PubMed

    Sajja, Yasodakrishna; Vulupala, Hanmanth Reddy; Bantu, Rajashaker; Nagarapu, Lingaiah; Vasamsetti, Sathish Babu; Kotamraju, Srigiridhar; Nanubolu, Jagadeesh Babu

    2016-02-01

    An efficient three-component protocol is described for the synthesis of benzo[6,7]cyclohepta[1,2-b]pyridine derivatives using β-chloroacroleins, 1,3-dicarbonyls and ammonium acetate under catalyst free conditions by using ethanol as reaction media. The mild reaction conditions, operational simplicity and high yields are the advantages of this protocol and the broad scope of this one-pot reaction makes this procedure promising for practical usages. All the final compounds were screened for anti-inflammatory activity. Among the compounds tested, the compounds 5a, 5b, 5c, 5d, 5f, and 5k exhibited significant inhibition of IL-1β and MCP-1 secretion as a measure of anti-inflammatory activity.

  18. One-pot system for synthesis, assembly, and display of functional single-span membrane proteins on oil-water interfaces.

    PubMed

    Yunker, Peter J; Asahara, Haruichi; Hung, Kuo-Chan; Landry, Corey; Arriaga, Laura R; Akartuna, Ilke; Heyman, John; Chong, Shaorong; Weitz, David A

    2016-01-19

    Single-span membrane proteins (ssMPs) represent approximately one-half of all membrane proteins and play important roles in cellular communications. However, like all membrane proteins, ssMPs are prone to misfolding and aggregation because of the hydrophobicity of transmembrane helices, making them difficult to study using common aqueous solution-based approaches. Detergents and membrane mimetics can solubilize membrane proteins but do not always result in proper folding and functionality. Here, we use cell-free protein synthesis in the presence of oil drops to create a one-pot system for the synthesis, assembly, and display of functional ssMPs. Our studies suggest that oil drops prevent aggregation of some in vitro-synthesized ssMPs by allowing these ssMPs to localize on oil surfaces. We speculate that oil drops may provide a hydrophobic interior for cotranslational insertion of the transmembrane helices and a fluidic surface for proper assembly and display of the ectodomains. These functionalized oil drop surfaces could mimic cell surfaces and allow ssMPs to interact with cell surface receptors under an environment closest to cell-cell communication. Using this approach, we showed that apoptosis-inducing human transmembrane proteins, FasL and TRAIL, synthesized and displayed on oil drops induce apoptosis of cultured tumor cells. In addition, we take advantage of hydrophobic interactions of transmembrane helices to manipulate the assembly of ssMPs and create artificial clusters on oil drop surfaces. Thus, by coupling protein synthesis with self-assembly at the water-oil interface, we create a platform that can use recombinant ssMPs to communicate with cells. PMID:26721399

  19. One-pot system for synthesis, assembly, and display of functional single-span membrane proteins on oil–water interfaces

    PubMed Central

    Yunker, Peter J.; Asahara, Haruichi; Hung, Kuo-Chan; Landry, Corey; Arriaga, Laura R.; Akartuna, Ilke; Heyman, John; Chong, Shaorong; Weitz, David A.

    2016-01-01

    Single-span membrane proteins (ssMPs) represent approximately one-half of all membrane proteins and play important roles in cellular communications. However, like all membrane proteins, ssMPs are prone to misfolding and aggregation because of the hydrophobicity of transmembrane helices, making them difficult to study using common aqueous solution-based approaches. Detergents and membrane mimetics can solubilize membrane proteins but do not always result in proper folding and functionality. Here, we use cell-free protein synthesis in the presence of oil drops to create a one-pot system for the synthesis, assembly, and display of functional ssMPs. Our studies suggest that oil drops prevent aggregation of some in vitro-synthesized ssMPs by allowing these ssMPs to localize on oil surfaces. We speculate that oil drops may provide a hydrophobic interior for cotranslational insertion of the transmembrane helices and a fluidic surface for proper assembly and display of the ectodomains. These functionalized oil drop surfaces could mimic cell surfaces and allow ssMPs to interact with cell surface receptors under an environment closest to cell–cell communication. Using this approach, we showed that apoptosis-inducing human transmembrane proteins, FasL and TRAIL, synthesized and displayed on oil drops induce apoptosis of cultured tumor cells. In addition, we take advantage of hydrophobic interactions of transmembrane helices to manipulate the assembly of ssMPs and create artificial clusters on oil drop surfaces. Thus, by coupling protein synthesis with self-assembly at the water–oil interface, we create a platform that can use recombinant ssMPs to communicate with cells. PMID:26721399

  20. One-pot synthesis of water-dispersible Ag2S quantum dots with bright fluorescent emission in the second near-infrared window

    NASA Astrophysics Data System (ADS)

    Yang, Hua-Yan; Zhao, Yu-Wei; Zhang, Zheng-Yong; Xiong, Huan-Ming; Yu, Shao-Ning

    2013-02-01

    The second near-infrared window (NIR-II, wavelength of 1.0-1.4 μm) is optimal for the bioimaging of live animals due to their low albedo and endogenous autofluorescence. Herein, we report a facile and one-pot biomimetic synthesis approach to prepare water-dispersible NIR-II-emitting ultrasmall Ag2S quantum dots (QDs). Photoluminescence spectra showed that the emission peaks could be tuned from 1294 to 1050 nm as the size of the Ag2S QDs varied from 6.8 to 1.6 nm. The x-ray diffraction patterns and x-ray photoelectron spectra confirmed that the products were monoclinic α-Ag2S. Fourier transform infrared spectrograph analysis indicated that the products were protein-conjugated Ag2S QDs. Examination of cytotoxicity and the hemolysis test showed that the obtained Ag2S QDs had good biocompatibility, indicating that such a nanomaterial could be a new kind of fluorescent label for in vivo imaging.

  1. One-pot synthesis of platinum-based nanoparticles incorporated into mesoporous niobium oxide-carbon composites for fuel cell electrodes.

    PubMed

    Orilall, M Christopher; Matsumoto, Futoshi; Zhou, Qin; Sai, Hiroaki; Abruña, Héctor D; DiSalvo, Francis J; Wiesner, Ulrich

    2009-07-01

    Catalyst-electrode design is crucial for the commercialization and widespread use of polymer electrolyte membrane fuel cells. There are considerable challenges in making less expensive, more durable, and more active catalysts. Herein, we report the one-pot synthesis of Pt and Pt-Pb nanoparticles incorporated into the pores of mesoporous niobium oxide-carbon composites. The self-assembly of block copolymers with niobium oxide and metal precursors results in an ordered mesostructured hybrid. Appropriate heat treatment of this hybrid produces highly crystalline, well-ordered mesoporous niobium oxide-carbon composites with Pt (or Pt-Pb) nanoparticles incorporated into the mesopores. The in situ-generated graphitic-like carbon material prevents the collapse of the mesostructure, while the metal oxide crystallizes at high temperatures and enhances the electrical conductivity of the final material. Formic acid electrooxidation with this novel material shows 4 times higher mass activities (3.3 mA/microg) and somewhat lower onset potentials (-0.24 V vs Ag/AgCl) than the best previously reported values employing Pt-Pb intermetallic nanoparticles supported on conducting carbon (0.85 mA/microg and -0.18 V, respectively).

  2. One-Pot Synthesis of CoSex -rGO Composite Powders by Spray Pyrolysis and Their Application as Anode Material for Sodium-Ion Batteries.

    PubMed

    Park, Gi Dae; Kang, Yun Chan

    2016-03-14

    A simple one-pot synthesis of metal selenide/reduced graphene oxide (rGO) composite powders for application as anode materials in sodium-ion batteries was developed. The detailed mechanism of formation of the CoSe(x)-rGO composite powders that were selected as the first target material in the spray pyrolysis process was studied. The crumple-structured CoSe(x)-rGO composite powders prepared by spray pyrolysis at 800 °C had a crystal structure consisting mainly of Co0.85 Se with a minor phase of CoSe2. The bare CoSe(x) powders prepared for comparison had a spherical shape and hollow structure. The discharge capacities of the CoSe(x)-rGO composite and bare CoSe(x) powders in the 50th cycle at a constant current density of 0.3 A g(-1) were 420 and 215 mA h g(-1), respectively, and their capacity retentions measured from the second cycle were 80 and 46%, respectively. The high structural stability of the CoSe(x)-rGO composite powders for repeated sodium-ion charge and discharge processes resulted in superior sodium-ion storage properties compared to those of the bare CoSe(x) powders.

  3. One-pot synthesis of N-F-Cr-doped anatase TiO₂ microspheres with nearly all-(001) surface for enhanced solar absorption.

    PubMed

    Wu, Jin-Ming; Tang, Mei-Lan

    2011-09-01

    The synthesis and clarifications in structure-property relationship for anatase TiO(2) crystals exposing (001) facets have attracted much attention. In this paper, a novel titania microsphere with nearly all-(001) surface was synthesized by hydrothermal treatment of a thermal sprayed TiN/Ti coating with HF aqueous solution containing chromium powders. Unlike the conventional (001)-facet exposed anatase crystals, which are highly truncated bipyramids, the crystal achieved in the current investigation is drum-like with a round cross section. The formation of the drum-like crystals was contributed to a balance between the erosion and precipitation of anatase single crystallites. The Cr-doping in anatase was believed to increase the surface deficiency which enhanced the erosion procedure, leading to the drum-like crystals. The XPS analysis confirmed the incorporations of N, F and Cr in the microsized anatase crystals through the one-pot reaction, which led to a significantly enhanced solar absorption. The UV-Vis diffuse reflectance revealed a band-to-band red-shift of the band gap of the anatase crystals to 1.60 eV, which is contributed mainly to the homogeneous Cr-doping. PMID:21847494

  4. Facile "one-pot" synthesis of poly(methacrylic acid)-based hybrid monolith via thiol-ene click reaction for hydrophilic interaction chromatography.

    PubMed

    Lv, Xumei; Tan, Wangming; Chen, Ye; Chen, Yingzhuang; Ma, Ming; Chen, Bo; Yao, Shouzhuo

    2016-07-01

    A novel sol-gel "one-pot" approach in tandem with a radical-mediated thiol-ene reaction for the synthesis of a methacrylic acid-based hybrid monolith was developed. The polymerization monomers, tetramethoxysilane (TMOS) and 3-mercaptopropyl trimethoxysilane (MPTS), were hydrolyzed in high-concentration methacrylic acid solution that also served as a hydrophilic functional monomer. The resulting solution was then mixed with initiator (2, 2'-azobis (2-methylpropionamide) dihydrochloride) and porogen (urea, polyethylene glycol 20,000) in a capillary column and polymerized in water bath. The column had a uniform porous structure and a good permeability. The evaluation of the monolith was performed by separation of small molecules including nucleosides, phenols, amides, bases and Triton X-100. The calibration curves for uridine, inosine, adenosine and cytidine were determined. All the calibration curves exhibited good linear regressions (R(2)≥0.995) within the test ranges of 0.5-40μg/mL for four nucleosides. Additionaliy, atypical hydrophilic mechanism was proved by elution order from low to high according to polarity retention time increased with increases in the content of the organic solvent in the mobile phase. Further studies indicated that hydrogen bond and electrostatic interactions existed between the polar analytes and the stationary phase. This was the mechanism of retention. The excellent separation of the BSA digest showed good hydrophility of the column and indicated the potential in separation of complex biological samples.

  5. Facile "one-pot" synthesis of poly(methacrylic acid)-based hybrid monolith via thiol-ene click reaction for hydrophilic interaction chromatography.

    PubMed

    Lv, Xumei; Tan, Wangming; Chen, Ye; Chen, Yingzhuang; Ma, Ming; Chen, Bo; Yao, Shouzhuo

    2016-07-01

    A novel sol-gel "one-pot" approach in tandem with a radical-mediated thiol-ene reaction for the synthesis of a methacrylic acid-based hybrid monolith was developed. The polymerization monomers, tetramethoxysilane (TMOS) and 3-mercaptopropyl trimethoxysilane (MPTS), were hydrolyzed in high-concentration methacrylic acid solution that also served as a hydrophilic functional monomer. The resulting solution was then mixed with initiator (2, 2'-azobis (2-methylpropionamide) dihydrochloride) and porogen (urea, polyethylene glycol 20,000) in a capillary column and polymerized in water bath. The column had a uniform porous structure and a good permeability. The evaluation of the monolith was performed by separation of small molecules including nucleosides, phenols, amides, bases and Triton X-100. The calibration curves for uridine, inosine, adenosine and cytidine were determined. All the calibration curves exhibited good linear regressions (R(2)≥0.995) within the test ranges of 0.5-40μg/mL for four nucleosides. Additionaliy, atypical hydrophilic mechanism was proved by elution order from low to high according to polarity retention time increased with increases in the content of the organic solvent in the mobile phase. Further studies indicated that hydrogen bond and electrostatic interactions existed between the polar analytes and the stationary phase. This was the mechanism of retention. The excellent separation of the BSA digest showed good hydrophility of the column and indicated the potential in separation of complex biological samples. PMID:27264742

  6. One pot synthesis of water-dispersible dehydroascorbic acid coated Fe3O4 nanoparticles under atmospheric air: blood cell compatibility and enhanced magnetic resonance imaging.

    PubMed

    Gupta, Hariom; Paul, P; Kumar, Naresh; Baxi, Seema; Das, Dipti P

    2014-09-15

    Water dispersible and biologically important molecule dehydroascorbic acid (DHA, capable to cross the blood brain barrier) coated Fe3O4 superparamagnetic nanoparticles having an average size of ∼6 nm were synthesized through one pot aqueous coprecipitation method under atmospheric air. An antioxidant ascorbic acid (AA) used in the synthesis oxidized itself to dehydroascorbic acid (DHA) to consume dissolved or available oxygen in reaction mixture which died away the oxidative impact of atmospheric air and formed DHA encapsulated the Fe3O4 nanoparticles which stabilized the Fe3O4 nanoparticles and significantly enhanced their colloidal solubility in water. Fe3O4 phase, superparamagnetic property, DHA coating and stable colloidal solubility in water were confirmed by means of XPS, VSM, IR and zeta potential analysis respectively. T1, T2 and T2(∗) weighted magnetic resonance imaging (MRI) and corresponding relaxivity (r1=0.416, r2=50.28 and r2(∗)=123.65 mM(-1) and r2/r1=120.86, r2(∗)r1=297.23) of colloidally dispersed DHA-coated nanoparticle water phantom revealed a strong contrast enhancement in T2 and T2(∗) weighted images. The compatibility of DHA-coated Fe3O4 nanoparticles toward human blood cells was examined by means of cell counting and cell morphological analysis with the use of optical microscope and scanning electron microscope imaging.

  7. One-pot synthesis of PEG modified BaLuF₅:Gd/Yb/Er nanoprobes for dual-modal in vivo upconversion luminescence and X-ray bioimaging.

    PubMed

    Rao, Ling; Lu, Wei; Zeng, Tianmei; Yi, Zhigao; Wang, Haibo; Liu, Hongrong; Zeng, Songjun

    2014-09-21

    Polyethylene glycol (PEG) modified BaLuF5:Gd/Yb/Er upconversion nanoparticles (UCNPs) were synthesized by a facile one-pot hydrothermal method for simultaneous synthesis and surface functionalization. The novel, excellently biocompatible and water-soluble bioprobes were used for simultaneous upconversion (UC) luminescence and X-ray bioimaging for the first time. The as-prepared BaLuF5:Gd/Yb/Er UCNPs possess a face-centered cubic structure with an average size of 23.7 ± 2.7 nm. Under 980 nm laser excitation, these UCNPs emitted intense UC luminescence via a two-photon process. In vitro bioimaging and localized luminescence spectra detected from HeLa cells and the background reveal that these UCNPs are ideal candidates for optical bioimaging in the absence of autofluorescence. Furthermore, the synergistic in vivo UC luminescence and X-ray bioimaging reveal that these PEG-modified BaLuF5:Gd/Yb/Er UCNPs can be successfully used as ideal dual-modal bioprobes. These results demonstrate that these PEG modified UCNPs are ideal multi-modal nanoprobes for bioimaging.

  8. One pot synthesis of nanosized anion doped TiO2: Effect of irradiation of sound waves on surface morphology and optical properties

    NASA Astrophysics Data System (ADS)

    Sharotri, Nidhi; Sud, Dhiraj

    2015-08-01

    Commercialization of AOP's for remediation of pollutants from environmental matrix required the process to be operated by solar light. Semiconductor TiO2 has emerged as an effective and preferred photocatalyst in the field of environmental photocatalysis due to its; (i) biological and chemical inertness (ii) resistance to chemical and photo corrosion, (iii) can absorb natural UV light due to appropriate energetic separation between its valence and conduction band. However, unfortunately the optical band gap of TiO2 (3.0-3.23 eV) with absorption cut off ˜ 380 nm, enables it to harness only a small fraction (˜ 5%) of the entire solar spectrum. One of the current areas of research is modification of TiO2 photocatalyst. In present paper one pot greener synthesis from titanium isopropoxide and hydroxylamine hydrochloride has been used as titanium and nitrogen precursor under ultrasonic waves. The as synthesized TiO2 nanomaterials were dried at 100°C and further calcinated at different temperatures. The effect of reaction parameters such as ultrasonication time on the yield, surface morphology, spectroscopic data and optical properties was also investigated. The results confirm that the anatase phase is a main phase with a crystallite size of 35-77 nm and the calculated band gap of nanomaterials varies from 2.10-3.1 eV.

  9. L-cysteine functionalized magnetic nanoparticles (LCMNP): a novel magnetically separable organocatalyst for one-pot synthesis of 2-amino-4H-chromene-3-carbonitriles in water.

    PubMed

    Khalafi-Nezhad, Ali; Nourisefat, Maryam; Panahi, Farhad

    2015-07-28

    In this study, L-cysteine was chemically grafted to magnetic nanoparticles in order to prepare a reusable magnetic material incorporating an amino acid moiety. For this purpose, silica-coated magnetic nanoparticles (Fe3O4@SiO2) were reacted with trimethoxy(vinyl)silane to produce vinyl-functionalized magnetic nanoparticles (VMNP). Reaction of a VMNP substrate with L-cysteine in the presence of azobisisobutyronitrile (AIBN) resulted in the production of L-cysteine-functionalized magnetic nanoparticles (LCMNP). The LCMNP material was characterized using different microscopy and spectroscopy techniques such as FT-IR, XRD, TEM, SEM, EDX, VSM, and elemental analysis. Also, LCMNP was analyzed by thermogravimetric analysis (TGA) in order to determine its thermal behavior. The applicability of the LCMNP material was evaluated in a three-component coupling reaction between a nucleophile, salicylaldehyde and malononitrile as the catalyst for one-pot synthesis of 2-amino-4H-chromene-3-carbonitrile derivatives. The catalyst system showed high catalytic activity in this process and target products were obtained in high isolated yields in water as a green solvent. The LCMNP catalyst was reusable in this reaction at least 7 times with no significant decrease in its catalytic activity.

  10. One-pot synthesis of ZnO2/ZnO composite with enhanced photocatalytic performance for organic dye removal.

    PubMed

    Liu, Wei; Wang, Mingliang; Xu, Chunxiang; Chen, Shifu; Fu, Xianliang

    2013-01-01

    The ZnO2/ZnO photocatalysts with various ZnO2 contents were prepared by one-pot synthesis method using ZnO and H2O2 as raw materials. The photocatalysts were characterized by XRD, UV-vis DRS, SEM, EDS, FT-IR spectra, fluorescence emission spectra, and BET specific area. The photocatalytic performance of the photocatalyst was evaluated by photocatalytic degradation of methyl orange (MO) and rhodamine B (RhB). The results showed that the photocatalytic activity of the ZnO2/ZnO was much higher than that of single-phase ZnO or ZnO2. The optimum ZnO2 content was 1.0 wt.%. The maximal degradation rate constant of MO and RhB was 4.1 times and 2.2 times that observed for pure ZnO, respectively. The stability of the prepared photocatalyst in the photocatalytic process was also investigated. The active species in dye degradation were examined by adding a series of scavengers. The possible mechanisms involved in the photocatalytic degradation of dye were also discussed.

  11. One pot synthesis of nanosized anion doped TiO{sub 2}: Effect of irradiation of sound waves on surface morphology and optical properties

    SciTech Connect

    Sharotri, Nidhi Sud, Dhiraj

    2015-08-28

    Commercialization of AOP’s for remediation of pollutants from environmental matrix required the process to be operated by solar light. Semiconductor TiO{sub 2} has emerged as an effective and preferred photocatalyst in the field of environmental photocatalysis due to its; (i) biological and chemical inertness (ii) resistance to chemical and photo corrosion, (iii) can absorb natural UV light due to appropriate energetic separation between its valence and conduction band. However, unfortunately the optical band gap of TiO{sub 2} (3.0-3.23 eV) with absorption cut off ∼ 380 nm, enables it to harness only a small fraction (∼ 5%) of the entire solar spectrum. One of the current areas of research is modification of TiO{sub 2} photocatalyst. In present paper one pot greener synthesis from titanium isopropoxide and hydroxylamine hydrochloride has been used as titanium and nitrogen precursor under ultrasonic waves. The as synthesized TiO{sub 2} nanomaterials were dried at 100°C and further calcinated at different temperatures. The effect of reaction parameters such as ultrasonication time on the yield, surface morphology, spectroscopic data and optical properties was also investigated. The results confirm that the anatase phase is a main phase with a crystallite size of 35-77 nm and the calculated band gap of nanomaterials varies from 2.10-3.1 eV.

  12. One-pot three-component domino protocol for the synthesis of novel pyrano[2,3-d]pyrimidines as antimicrobial and anti-biofilm agents.

    PubMed

    Suresh, Lingala; Poornachandra, Y; Kanakaraju, S; Ganesh Kumar, C; Chandramouli, G V P

    2015-07-14

    A simple and facile synthesis of a series of novel pyrano[2,3-d]pyrimidines has been achieved successfully via the one-pot three-component reaction of 2-amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[4,3-b]pyran-3-carbonitriles, DMF-DMA and arylamines in the presence of 1-butyl-3-methylhydrogensulphate [Bmim]HSO4 ionic liquid. This method has several advantages such as high yields, clean reaction, simple methodology and short reaction times. The synthesized compounds were evaluated for their antimicrobial activity against Gram-positive, Gram-negative and different Candida strains. Among the derivatives screened, compounds 4c, 4d, 4h and 4l were found to be active against both bacterial and Candida strains with MIC values ranging from 3.9 to 31.2 μg mL(-1). In addition, compound 4l showed a good minimum bactericidal concentration, minimum fungicidal concentration and anti-biofilm activities. Furthermore, the mode of the antifungal action for the promising compound 4l was evaluated in C. albicans MTCC 1637 through an ergosterol biosynthesis inhibition process.

  13. One-pot synthesis of podophyllotoxin-thiourea congeners by employing NH₂SO₃H/NaI: Anticancer activity, DNA topoisomerase-II inhibition, and apoptosis inducing agents.

    PubMed

    Shankaraiah, Nagula; Kumar, Niggula Praveen; Amula, Suresh Babu; Nekkanti, Shalini; Jeengar, Manish Kumar; Naidu, V G M; Reddy, T Srinivasa; Kamal, Ahmed

    2015-10-01

    A facile one-pot method for the synthesis of novel podophyllotoxin-thiourea congeners has been developed by using NH2SO3H/NaI system. Interestingly, 4β-azido podophyllotoxin reduction with concomitant aryl isothiocyanates coupling under mild reaction conditions has been achieved. These compounds have been investigated for their in vitro cytotoxicity against A549, MDA MB-231, DU-145, LNCaP, and HGC-27 cancer cell lines. Some of the representative compounds have selectively exhibited cytotoxicity on DU-145 (human prostate cancer) cells and the most potent compound was 4a (IC50 of 0.50 ± 0.03 μM) with optimal safety therapeutic window (81.7 fold) on normal human prostate cell line (RWPE-1, IC50 of 40.85 ± 0.78). The flow-cytometric analysis of the compound 4a in prostate cancer cells indicated a strong G2/M-phase arrest and significant topoisomerase II inhibition activity. Furthermore, these compounds induce apoptosis as observed by Acridine Orange and Ethidium Bromide (AO/EB) staining and Annexin V binding assay. Molecular docking results of the title compounds with topoisomerase-IIα were presented as theoretical support for the experimental data.

  14. A facile one-pot synthesis of 2-arylamino-5-aryloxylalkyl-1,3,4-oxadiazoles and their urease inhibition studies.

    PubMed

    Akhtar, Tashfeen; Khan, Muhammad A; Iqbal, Jamshed; Jones, Peter G; Hameed, Shahid

    2014-07-01

    A one-pot method for the synthesis of structural type urease inhibitors, 2-amino-1,3,4-oxadiazoles, was developed. The structures of the compounds were established using spectroanalytical techniques and unambiguously confirmed by single-crystal X-ray analysis of compound 3o. The synthesized compounds were tested against jack beans urease, and most of the compounds (3c, 3g, 3j, 3k, 3n, 3r-3v) were found more active than the standard. The most potent compound (3u) had an IC50 value of 6.03 ± 0.02 μm as compared to the IC50 value of the standard (thiourea; 22.0 ± 1.2 μm). The prominent urease inhibition activity of these compounds may serve as an important finding in the development of less toxic and more potent antiulcer drugs. The compounds were also investigated against four bacterial strains, and some of the compounds (3g and 3r) were found more potent than the standard drug (ciprofloxacin) against all the tested strains. The MIC value for compound 3g was 0.156 μmol/mL against the tested bacterial strains.

  15. Synthesis of antiproliferative 13α-d-homoestrones via Lewis acid-promoted one-pot Prins-Ritter reactions of d-secosteroidal δ-alkenyl-aldehydes.

    PubMed

    Huber, Judit; Wölfling, János; Schneider, Gyula; Ocsovszki, Imre; Varga, Mónika; Zupkó, István; Mernyák, Erzsébet

    2015-10-01

    A simple one-pot Prins-Ritter route was developed for the synthesis of 16-acylamino-17a-hydroxy-d-homoestrone 3-benzyl and 3-methyl ethers in the 13α-estrone series. The d-secosteroidal δ-alkenyl-aldehydes were allowed to react with different nitriles in the presence of BF3·OEt2 as a Lewis acid catalyst. Prins cyclizations afforded 17a-hydroxy-16-carbenium ions, which underwent Ritter reactions with nitriles, leading to 16α- or 16β-acylamino derivatives. A side-product in which a dihydro-1,3-oxazine was bridged to six-membered ring D at positions 16α,17aα was formed in each reaction. The antiproliferative properties of the novel 13α-d-homosteroids were determined on a panel of human adherent cancer cell lines (HeLa, MCF-7, T47D, MDA-MB-231, MDA-MB-361, A2780 and A431) by means of MTT (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyltetrazolium bromide) assays. Some compounds proved to be more effective (with submicromolar IC50 values) than the reference agent cisplatin. One of the most potent compounds substantially increased the rate of tubulin polymerization. Cell cycle analyses by flow cytometry indicated a concentration-dependent accumulation of the G2/M cell population.

  16. One-pot synthesis, biological evaluation, and docking study of new chromeno-annulated thiopyrano[2,3-c]pyrazoles.

    PubMed

    Parmar, Bhagyashri D; Sutariya, Tushar R; Brahmbhatt, Gaurangkumar C; Parmar, Narsidas J; Kant, Rajni; Gupta, Vivek K; Murumkar, Prashant R; Sharma, Mayank Kumar; Yadav, Mange Ram

    2016-08-01

    A one-pot synthesis of new chromeno-annulated thiopyrano[2,3-c]pyrazoles has been achieved through a domino-Knoevenagel-hetero-Diels-Alder reaction after combining various pyrazol-5-thiones with O-alkenyloxy/alkynyloxy-salicylaldehydes/naphthaldehydes in a Brønsted acidic ionic liquid, [Hmim]HSO[Formula: see text], methylimidazolium hydrogen sulphate, under microwave irradiation. The method is simple and in many cases the isolated products did not require further purification. The central pyranothiopyranyl cis-fusion was confirmed by 2D NMR NOESY and single-crystal X-ray analysis suggesting that the endo-E-Syn transition state would be the most favored pathway of the reaction. Many heterocycles of this new series were found active against six bacterial and two fungal strains. In addition, all the compounds possess good anti-oxidant activity with the ferric reducing anti-oxidant power value [Formula: see text]. All new structures were docked into active site of angiotensin I converting enzyme (ACE), assuming that the compounds possessed the anti-hypertensive activity potential on the basis of prediction of activity spectra of substances prediction results. Pyranyl ring oxygen in compound 9a forms two hydrogen bonds with HIS353 and HIS513 residues in the active site of the ACE having good G score ([Formula: see text]) of this compound, comparable to that of the reference drug captopril ([Formula: see text]). PMID:27017351

  17. Facile one-pot synthesis of organic dye-complexed microgels for optical detection of glucose at physiological pH.

    PubMed

    Li, Yingyu; Zhou, Shuiqin

    2013-06-21

    With a rational design of functional co-monomers, low-cost dye-complexed microgels, capable of continuous glucose detection at physiological pH, were readily synthesized in one-pot via precipitation polymerization in water.

  18. A one-pot protocol for synthesis of non-noble metal-based core-shell nanoparticles under ambient conditions: toward highly active and cost-effective catalysts for hydrolytic dehydrogenation of NH3BH3.

    PubMed

    Jiang, Hai-Long; Akita, Tomoki; Xu, Qiang

    2011-10-21

    A one-pot synthesis of non-noble transition metal-based core-shell nanoparticles (NPs) has been developed under ambient conditions. The obtained Cu@M (M = Co, Fe, Ni) NPs exhibit superior catalytic activity for hydrolytic dehydrogenation of NH(3)BH(3), compared to the alloy and monometallic counterparts. PMID:21909589

  19. An enantioselective strategy for the total synthesis of (S)-tylophorine via catalytic asymmetric allylation and a one-pot DMAP-promoted isocyanate formation/Lewis acid catalyzed cyclization sequence.

    PubMed

    Su, Bo; Zhang, Hui; Deng, Meng; Wang, Qingmin

    2014-06-14

    A new asymmetric total synthesis of a phenanthroindolizidine alkaloid (S)-tylophorine is reported, which features a catalytic asymmetric allylation of aldehydes and an unexpected one-pot DMAP promoted isocyanate formation and Lewis acid catalyzed intramolecular cyclization reaction. In addition, White's direct C-H oxidation catalyst system converting monosubstituted olefins to linear allylic acetates was also employed for late-stage transformation.

  20. A Green, Expeditious, One-Pot Synthesis of 3, 4-Dihydropyrimidin-2(1H)-ones Using a Mixture of Phosphorus Pentoxide-Methanesulfonic Acid at Ambient Temperature

    PubMed Central

    Borse, Amulrao; Patil, Mahesh; Patil, Nilesh; Shinde, Rohan

    2012-01-01

    An expeditious, one-pot method for the synthesis of 3,4-dihydropyrimidin-2(1H)-ones using a mixture of phosphorus pentoxide-methanesulfonic acid (Eaton's reagent) at room temperature under solvent-free conditions is described. The salient features of this method include short reaction time, green aspects, high yields, and simple procedure. PMID:24052843

  1. One-pot synthesis of silica-hybridized Ag{sub 2}S–CuS nanocomposites with tunable nonlinear optical properties

    SciTech Connect

    Ann Mary, K.A.; Unnikrishnan, N.V.; Philip, Reji

    2015-10-15

    Highlights: • Silica modified QDs of CuS and Ag{sub 2}S is developed at room temperature. • Formation of Ag{sub 2}S/CuS nanocomposites is confirmed from XRD and FFT of HRTEM images. • The concentration dependent growth of silica modified QDs is discussed. • Nonlinear absorption observed in ns excitations is dominated by SA and ESA. • Tuning of optical limiting efficiency is achieved with relative Ag{sub 2}S content. - Abstract: In the present work we report a simple, facile route developed for preparing silica hybridized copper sulfide and silver sulfide quantum dots at room temperature. By adjusting the concentration of the precursors, Ag{sub 2}S can form Ag{sub 2}S–CuS nanocomposites which are self regulated in one pot. Their crystalline, structural and optical properties have been investigated in detail, and the optical limiting nature is studied from fluence-dependent transmittance measurements employing short (5 ns) laser pulses at 532 nm. Ag{sub 2}S nanoparticles are found to have large third order nonlinear optical coefficients with a relatively lower optical limiting threshold of 1.7 J cm{sup −2}, while the nonlinearity of the nanocomposites is found to lie in between that of Ag{sub 2}S and CuS nanoparticles. These results suggest pathways for designing good quality optical limiters with tunable optical limiting efficiencies by varying the constituent nanocrystal compositions.

  2. One-pot synthesis of phenylmethanethiolate-protected Au20(SR)16 and Au24(SR)20 nanoclusters and insight into the kinetic control.

    PubMed

    Zhu, Xiuyi; Jin, Shenshen; Wang, Shuxin; Meng, Xiangming; Zhu, Changwei; Zhu, Manzhou; Jin, Rongchao

    2013-11-01

    We report two synthetic routes for concurrent formation of phenylmethanethiolate (-SCH2Ph)-protected Au20(SR)16 and Au24(SR)24 nanoclusters in one-pot by kinetic control. Unlike the previously reported methods for thiolate-protected gold nanoclusters, which typically involve rapid reduction of the gold precursor by excess NaBH4 and subsequent size focusing into atomically monodisperse clusters of a specific size, the present work reveals some insight into the kinetic control in gold-thiolate cluster synthesis. We demonstrate that the synthesis of -SCH2Ph-protected Au20 and Au24 nanoclusters can be obtained through two different, kinetically controlled methods. Specifically, route 1 employs slow addition of a relatively large amount of NaBH4 under slow stirring of the reaction mixture, while route 2 employs rapid addition of a small amount of NaBH4 under rapid stirring of the reaction mixture. At first glance, these two methods apparently possess quite different reaction kinetics, but interestingly they give rise to exactly the same product (i.e., the coproduction of Au20(SCH2Ph)16 and Au24(SCH2Ph)20 clusters). Our results explicitly demonstrate the complex interplay between the kinetic factors that include the addition speed and amount of NaBH4 solution as well as the stirring speed of the reaction mixture. Such insight is important for devising synthetic routes for different sized nanoclusters. We also compared the photoluminescence and electrochemical properties of PhCH2S-protected Au20 and Au24 nanoclusters with the PhC2H4S-protected counterparts. A surprising 2.5 times photoluminescence enhancement was observed for the PhCH2S-capped nanoclusters when compared to the PhC2H4S-capped analogues, thereby indicating a drastic effect of the ligand that is merely one carbon shorter.

  3. Polyallylamine functionalized palladium icosahedra: one-pot water-based synthesis and their superior electrocatalytic activity and ethanol tolerant ability in alkaline media.

    PubMed

    Fu, Gengtao; Jiang, Xian; Tao, Lin; Chen, Yu; Lin, Jun; Zhou, Yiming; Tang, Yawen; Lu, Tianhong

    2013-04-01

    Polyallylamine (PAH) functionalized Pd icosahedra are synthesized through a simple, one-pot, seedless and hydrothermal growth method. Herein, PAH is used efficiently as a complex-forming agent, capping agent, and facet-selective agent. The strong interaction between PAH and Pd atom sharply changes the electronic structure of Pd atom in the Pd icosahedra. The protective function of PAH layers and enhanced antietching capability of Pd atom are responsible for the formation of the Pd icosahedra. Very importantly, the as-prepared PAH functionalized Pd icosahedra exhibit superior electrocatalytic activity and ethanol tolerant ability toward the oxygen reduction reaction (ORR) compared to the commercially available Pt black in alkaline media. At 0.95 V (vs RHE), the ORR specific kinetic current density at the Pd icosahedra is 4.48 times higher than that at commercial Pt black. The fact demonstrates the appropriate surface modification of the Pd nanoparticles by nonmetallic molecules can be regarded as an effective way to enhance the electrocatalytic activity toward the ORR.

  4. One-pot hydrothermal synthesis of CuBi co-doped mesoporous zeolite Beta for the removal of NOx by selective catalytic reduction with ammonia.

    PubMed

    Xie, Zhiguo; Zhou, Xiaoxia; Wu, Huixia; Chen, Lisong; Zhao, Han; Liu, Yan; Pan, Linyu; Chen, Hangrong

    2016-01-01

    A series of CuBi co-doped mesoporous zeolite Beta (CuxBiy-mBeta) were prepared by a facile one-pot hydrothermal treatment approach and were characterized by XRD, N2 adsorption-desorption, TEM/SEM, XPS, H2-TPR, NH3-TPD and in situ DRIFTS. The catalysts CuxBiy-mBeta were applied to the removal of NOx by selective catalytic reduction with ammonia (NH3-SCR), especially the optimized Cu1Bi1-mBeta achieved the high efficiency for the removal of NOx and N2 selectivity, superior water and sulfur resistance as well as good durability. The excellent catalytic performance could be attributed to the acid sites of the support and the synergistic effect between copper and bismuth species. Moreover, in situ DRIFTS results showed that amides NH2 and NH4(+) generated from NH3 adsorption could be responsible for the high selective catalytic reduction of NOx to N2. In addition, a possible catalytic reaction mechanism on Cu1Bi1-mBeta for the removal of NOx by NH3-SCR was proposed for explaining this catalytic process. PMID:27445009

  5. One-pot synthesis of Ag/r-GO/TiO2 nanocomposites with high solar absorption and enhanced anti-recombination in photocatalytic applications.

    PubMed

    Gao, Weiyin; Wang, Minqiang; Ran, Chenxin; Yao, Xi; Yang, Honghui; Liu, Jing; He, Delong; Bai, Jinbo

    2014-05-21

    In this paper, we reported a simple one-pot solvothermal approach to fabricate Ag/reduced graphene oxide (r-GO)/TiO2 composite photocatalyst under atmospheric pressure. Based on the experimental data, we concluded that the introduction of Ag into classical graphene-TiO2 system (i) efficiently enlarges the absorption range, (ii) improves photogenerated electron separation and (iii) increases photocatalysis reaction sites. The optimized sample exhibits prominent photocatalysis ability as compared to pure TiO2 under simulated sunlight. We further proposed that besides the above three advantages of Ag, a different size of Ag nanoparticles is also responsible for the improved photocatalysis ability, where small size Ag nanoparticles (2-5 nm) could store a photoexcited electron that was generated from TiO2, while large-size Ag nanoparticles could utilize visible light due to their localized surface plasmon resonance (LSPR) absorption. Our present work gives new insights into the photocatalysis mechanism of noble metal/r-GO/TiO2 composites and provides a new pathway into the design of TiO2-based photocatalysts and promote their practical application in various environmental and energy issues.

  6. One-pot multi-component synthesis of 1,4-dihydropyridines using Zn(2+) @KSF and evaluating their antibacterial and antioxidant activities.

    PubMed

    Mahmoodi, Nosrat O; Ramzanpour, Sahar; Ghanbari Pirbasti, Fateme

    2015-04-01

    New 5-aryl-10-(4-(4-methoxyphenyl)thiazole-2-yl)-9,10-dihydropyrido[2,3-d:5,6-d']dipyrimidinone-2,4,6,8-(1H,3H,5H,7H)-tetraones 6a-d were synthesized through one-pot four-component reaction of aldehydes, barbituric acid, and thiazole using Zn(2+) @KSF under reflux condition. The key features of this reaction are: incorporating four heterocyclic rings, using a heterogeneous and efficient catalyst, high yield, and easy-to-setup reaction. The structure of the products was confirmed by FT-IR, (1)H NMR, and (13)C NMR spectra. The antibacterial activities of compounds 6a-d were screened against Escherichia coli, Micrococcus luteus, Pseudomonas aeruginosa, and Staphylococcus aureus bacterial strains using the zone inhibition method. Also, the 2,2-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activities of compounds 6a-d were evaluated. All compounds showed good antioxidant capacity in comparison to ascorbic acid. The IC50 values of the antioxidant activity were calculated. The proposed mechanism for antioxidant activity is discussed.

  7. One-pot hydrothermal synthesis of CuBi co-doped mesoporous zeolite Beta for the removal of NOx by selective catalytic reduction with ammonia.

    PubMed

    Xie, Zhiguo; Zhou, Xiaoxia; Wu, Huixia; Chen, Lisong; Zhao, Han; Liu, Yan; Pan, Linyu; Chen, Hangrong

    2016-07-22

    A series of CuBi co-doped mesoporous zeolite Beta (CuxBiy-mBeta) were prepared by a facile one-pot hydrothermal treatment approach and were characterized by XRD, N2 adsorption-desorption, TEM/SEM, XPS, H2-TPR, NH3-TPD and in situ DRIFTS. The catalysts CuxBiy-mBeta were applied to the removal of NOx by selective catalytic reduction with ammonia (NH3-SCR), especially the optimized Cu1Bi1-mBeta achieved the high efficiency for the removal of NOx and N2 selectivity, superior water and sulfur resistance as well as good durability. The excellent catalytic performance could be attributed to the acid sites of the support and the synergistic effect between copper and bismuth species. Moreover, in situ DRIFTS results showed that amides NH2 and NH4(+) generated from NH3 adsorption could be responsible for the high selective catalytic reduction of NOx to N2. In addition, a possible catalytic reaction mechanism on Cu1Bi1-mBeta for the removal of NOx by NH3-SCR was proposed for explaining this catalytic process.

  8. One-pot hydrothermal synthesis of CuBi co-doped mesoporous zeolite Beta for the removal of NOx by selective catalytic reduction with ammonia

    NASA Astrophysics Data System (ADS)

    Xie, Zhiguo; Zhou, Xiaoxia; Wu, Huixia; Chen, Lisong; Zhao, Han; Liu, Yan; Pan, Linyu; Chen, Hangrong

    2016-07-01

    A series of CuBi co-doped mesoporous zeolite Beta (CuxBiy-mBeta) were prepared by a facile one-pot hydrothermal treatment approach and were characterized by XRD, N2 adsorption-desorption, TEM/SEM, XPS, H2-TPR, NH3-TPD and in situ DRIFTS. The catalysts CuxBiy-mBeta were applied to the removal of NOx by selective catalytic reduction with ammonia (NH3-SCR), especially the optimized Cu1Bi1-mBeta achieved the high efficiency for the removal of NOx and N2 selectivity, superior water and sulfur resistance as well as good durability. The excellent catalytic performance could be attributed to the acid sites of the support and the synergistic effect between copper and bismuth species. Moreover, in situ DRIFTS results showed that amides NH2 and NH4+ generated from NH3 adsorption could be responsible for the high selective catalytic reduction of NOx to N2. In addition, a possible catalytic reaction mechanism on Cu1Bi1-mBeta for the removal of NOx by NH3-SCR was proposed for explaining this catalytic process.

  9. One-pot hydrothermal synthesis of CuBi co-doped mesoporous zeolite Beta for the removal of NOx by selective catalytic reduction with ammonia

    PubMed Central

    Xie, Zhiguo; Zhou, Xiaoxia; Wu, Huixia; Chen, Lisong; Zhao, Han; Liu, Yan; Pan, Linyu; Chen, Hangrong

    2016-01-01

    A series of CuBi co-doped mesoporous zeolite Beta (CuxBiy-mBeta) were prepared by a facile one-pot hydrothermal treatment approach and were characterized by XRD, N2 adsorption-desorption, TEM/SEM, XPS, H2-TPR, NH3-TPD and in situ DRIFTS. The catalysts CuxBiy-mBeta were applied to the removal of NOx by selective catalytic reduction with ammonia (NH3-SCR), especially the optimized Cu1Bi1-mBeta achieved the high efficiency for the removal of NOx and N2 selectivity, superior water and sulfur resistance as well as good durability. The excellent catalytic performance could be attributed to the acid sites of the support and the synergistic effect between copper and bismuth species. Moreover, in situ DRIFTS results showed that amides NH2 and NH4+ generated from NH3 adsorption could be responsible for the high selective catalytic reduction of NOx to N2. In addition, a possible catalytic reaction mechanism on Cu1Bi1-mBeta for the removal of NOx by NH3-SCR was proposed for explaining this catalytic process. PMID:27445009

  10. Heterogeneous ceria catalyst with water-tolerant Lewis acidic sites for one-pot synthesis of 1,3-diols via Prins condensation and hydrolysis reactions.

    PubMed

    Wang, Yehong; Wang, Feng; Song, Qi; Xin, Qin; Xu, Shutao; Xu, Jie

    2013-01-30

    The use of a heterogeneous Lewis acid catalyst, which is insoluble and easily separable during the reaction, is a promising option for hydrolysis reactions from both environmental and practical viewpoints. In this study, ceria showed excellent catalytic activity in the hydrolysis of 4-methyl-1,3-dioxane to 1,3-butanediol in 95% yield and in the one-pot synthesis of 1,3-butanediol from propylene and formaldehyde via Prins condensation and hydrolysis reactions in an overall yield of 60%. In-depth investigations revealed that ceria is a water-tolerant Lewis acid catalyst, which has seldom been reported previously. The ceria catalysts showed rather unusual high activity in hydrolysis, with a turnover number (TON) of 260, which is rather high for bulk oxide catalysts, whose TONs are usually less than 100. Our conclusion that ceria functions as a Lewis acid catalyst in hydrolysis reactions is firmly supported by thorough characterizations with IR and Raman spectroscopy, acidity measurements with IR and (31)P magic-angle-spinning NMR spectroscopy, Na(+)/H(+) exchange tests, analyses using the in situ active-site capping method, and isotope-labeling studies. A relationship between surface vacancy sites and catalytic activity has been established. CeO(2)(111) has been confirmed to be the catalytically active crystalline facet for hydrolysis. Water has been found to be associatively adsorbed on oxygen vacancy sites with medium strength, which does not lead to water dissociation to form stable hydroxides. This explains why the ceria catalyst is water-tolerant. PMID:23228093

  11. One-pot synthesis of hierarchical Ni2P/MoS2 hybrid electrocatalysts with enhanced activity for hydrogen evolution reaction

    NASA Astrophysics Data System (ADS)

    Liu, Yan-Ru; Hu, Wen-Hui; Li, Xiao; Dong, Bin; Shang, Xiao; Han, Guan-Qun; Chai, Yong-Ming; Liu, Yun-Qi; Liu, Chen-Guang

    2016-10-01

    A simple one-pot synthesis method has been used to fabricate novel Ni2P/MoS2 hybrid electrocatalysts for hydrogen evolution reaction (HER). Owing to the weak conductivity and layered structure of MoS2, Ni2P nanoparticles with excellent conductivity and activity have been doped into MoS2 for improving the electrocatalytic performances for HER. The structure and morphology of the as-prepared Ni2P/MoS2 hybrid nanostructures are characterized. XRD and XPS show the elemental composition and valence of Ni2P/MoS2. SEM and TEM confirm that the close interaction of the hybrid materials and good dispersion of Ni2P nanoparticles. The as-synthesized Ni2P/MoS2 hybrid electrocatalysts exhibit excellent activity with onset overpotential of 75 mV and Tafle slope of 76 mV dec-1, which are much better than that of pure MoS2. The enhanced stability of the as-prepared Ni2P/MoS2 for HER has also been observed. The improved performances for HER may be ascribed to the better conductivity and dispersion of MoS2 nanosheets in Ni2P/MoS2 hybrid electrocatalysts. The small size and good dispersion of Ni2P nanoparticles also contributed to the enhancement of HER activity. Compared with mechanically mixed MoS2 and Ni2P (Ni2P-MoS2), Ni2P/MoS2 hybrid materials demonstrate better electrochemical performances for HER, implying the existence of synergistic effect between Ni2P and MoS2 on HER activity.

  12. One-Pot Polyol Synthesis of Pt/CeO2 and Au/CeO2 Nanopowders as Catalysts for CO Oxidation.

    PubMed

    Pilger, Frank; Testino, Andrea; Lucchini, Mattia Alberto; Kambolis, Anastasios; Tarik, Mohammed; El Kazzi, Mario; Arroyo, Yadira; Rossell, Marta D; Ludwig, Christian

    2015-05-01

    The facile one-pot synthesis of CeO2-based catalysts has been developed to prepare a relatively large amount of nanopowders with relevant catalytic activity towards CO oxidation. The method consists of a two-steps process carried out in ethylene glycol: in the first step, 5 nm well-crystallized pure CeO2 is prepared. In a subsequent second step, a salt of a noble metal is added to the CeO2 suspension and the deposition of the noble metal on the nanocrystalline CeO2 is induced by heating. Two catalysts were prepared: Pt/CeO2 and Au/CeO2. The as-prepared catalysts, the thermally treated catalysts, as well as the pure CeO2, are characterized by XRD, TGA, XPS, FTIR, HR-TEM, STEM, particle size distribution, and N2-physisorption. In spite of the identical preparation protocol, Au and Pt behave in a completely different way: Au forms rather large particles, most of them with triangular shape, easily identifiable and dispersed in the CeO2 matrix. In contrast, Pt was not identified as isolated particles. The high resolution X-ray diffraction carried out on the Pt/CeO2 thermally treated sample (500 degrees C for 1 h) shows a significant CeO2 lattice shrinkage, which can be interpreted as an at least partial incorporation of Pt into the CeO2 crystal lattice. Moreover, only Pt2+ and Pt4+ species were identified by XPS. In literature, the incorporation of Pt into the CeO2 lattice is supported by first-principle calculations and experimentally demonstrated only by combustion synthesis methods. To the best of our knowledge this is the first report where ionically dispersed Pt into the CeO2 lattice is obtained via a liquid synthesis method. The thermally treated Pt/CeO2 sample revealed good activity with 50% CO conversion at almost room temperature.

  13. One-pot facile synthesis of reusable tremella-like M1@M2@M1(OH)2 (M1 = Co, Ni, M2 = Pt/Pd, Pt, Pd and Au) three layers core-shell nanostructures as highly efficient catalysts.

    PubMed

    Liu, Yadong; Fang, Zhen; Kuai, Long; Geng, Baoyou

    2014-08-21

    In this work, a general, facile, successive and eco-friendly method for multilayer nanostructures has been established for the first time. We take full advantage of the structural and compositional character of M1@M2 (M1 = Co, Ni, M2 = Pt/Pd, Pt, Pd and Au) core-shell nanostructures to prepare a series of reusable tremella-like M1@M2@M1(OH)2 three layer core-shell or yolk-shell nanocomposites with a magnetic core, a porous noble metal shell, and an ultrathin cobalt or nickel hydroxide shell. We evaluated their catalytic performance using a model reaction based on the reduction of 4-nitrophenol. These novel M1@M2@M1(OH)2 nanomaterials with a unique internal micro environment promoted the efficiency of the catalytic reaction, prolonged the service life of the catalyst and enhanced the overall activity of the catalyst in the catalytic process. The novel three layer core-shell nanocomposites can be extended to other applications such as biomedical detection, energy conversion and storage systems. PMID:25008373

  14. Traceless OH-Directed Wacker Oxidation-Elimination, an Alternative to Wittig Olefination/Aldol Condensation: One-Pot Synthesis of α,β-Unsaturated and Nonconjugated Ketones from Homoallyl Alcohols.

    PubMed

    Bethi, Venkati; Fernandes, Rodney A

    2016-09-16

    A new method for one-pot synthesis of β-substituted and β,β-disubstituted α,β-unsaturated methyl ketones from homoallyl alcohols by sequential PdCl2/CrO3-promoted Wacker process followed by an acid-mediated dehydration reaction has been developed. Remarkably, internal homoallyl alcohols delivered regioselectively nonconjugated unsaturated carbonyl compounds under the same protocol. A new starting material-based synthesis of α,β-unsaturated and nonconjugated methyl ketones is demonstrated.

  15. One-Pot Aminoethylation of Indoles/Pyrroles with Alkynes and Sulfonyl Azides.

    PubMed

    Rajasekar, Shanmugam; Yadagiri, Dongari; Anbarasan, Pazhamalai

    2015-11-16

    A general and efficient one-pot aminoethylation of substituted indoles/pyrroles was accomplished for the synthesis of various tryptamine derivatives employing a combination of alkynes and sulfonyl azides as readily accessible aminoethylating agents. The reaction features a successful integration of copper-catalyzed alkyne and azide cycloaddition to N-sulfonyl-1,2,3-triazole, rhodium-catalyzed selective insertion of α-iminocarbenes onto the C3-H bond of indoles, and reduction of the resultant enamides to tryptamine derivatives employing either NaCNBH3 or palladium catalyst, in one-pot. The reaction also showed excellent functional-group tolerance and allowed the synthesis of various substituted tryptamines in good to excellent yield. This transformation constitutes a one-pot formal regioselective functionalization of terminal alkynes. Utility of the synthesized tryptamine was further demonstrated in the synthesis of dihydro-β-carboline and tryptoline. PMID:26443500

  16. One-Pot Aminoethylation of Indoles/Pyrroles with Alkynes and Sulfonyl Azides.

    PubMed

    Rajasekar, Shanmugam; Yadagiri, Dongari; Anbarasan, Pazhamalai

    2015-11-16

    A general and efficient one-pot aminoethylation of substituted indoles/pyrroles was accomplished for the synthesis of various tryptamine derivatives employing a combination of alkynes and sulfonyl azides as readily accessible aminoethylating agents. The reaction features a successful integration of copper-catalyzed alkyne and azide cycloaddition to N-sulfonyl-1,2,3-triazole, rhodium-catalyzed selective insertion of α-iminocarbenes onto the C3-H bond of indoles, and reduction of the resultant enamides to tryptamine derivatives employing either NaCNBH3 or palladium catalyst, in one-pot. The reaction also showed excellent functional-group tolerance and allowed the synthesis of various substituted tryptamines in good to excellent yield. This transformation constitutes a one-pot formal regioselective functionalization of terminal alkynes. Utility of the synthesized tryptamine was further demonstrated in the synthesis of dihydro-β-carboline and tryptoline.

  17. Multicapillary Flow Reactor: Synthesis of 1,2,5-Thiadiazepane 1,1-Dioxide Library Utilizing One-Pot Elimination and Inter-/Intramolecular Double aza-Michael Addition Via Microwave-Assisted, Continuous-Flow Organic Synthesis (MACOS)

    PubMed Central

    Ullah, Farman; Zang, Qin; Javed, Salim; Zhou, Aihua; Knudtson, Christopher A.; Bi, Danse; Hanson, Paul R.; Organ, Michael G.

    2013-01-01

    A microwave-assisted, continuous-flow organic synthesis (MACOS) protocol for the synthesis of functionalized 1,2,5-thiadiazepane 1,1-dioxide library, utilizing a one-pot elimination and inter-/intramolecular double aza-Michael addition strategy is reported. The optimized protocol in MACOS was utilized for scale-out and further extended for library production using a multicapillary flow reactor. A 50-member library of 1,2,5-thiadiazepane 1,1-dioxides was prepared on a 100- to 300-mg scale with overall yields between 50 and 80% and over 90 % purity determined by proton nuclear magnetic resonance (1H-NMR) spectroscopy. PMID:24244871

  18. One-pot approach to 1,2-disubstituted indoles via Cu(II)-catalyzed coupling/cyclization under aerobic conditions and its application for the synthesis of polycyclic indoles.

    PubMed

    Gao, Jilong; Shao, Yingying; Zhu, Jiaoyan; Zhu, Jiaqi; Mao, Hui; Wang, Xiaoxia; Lv, Xin

    2014-10-01

    A straightforward assembly of 1,2-disubstituted indoles has been developed through a Cu(II)-catalyzed domino coupling/cyclization process. Under aerobic conditions, a wide range of 1,2-disubstituted indole derivatives were efficiently and facilely synthesized from 2-alkynylanilines and boronic acids. 2-(2-Bromoaryl)-1-aryl-1H-indoles, which were selectively generated in one pot under the Cu catalysis, afforded the indolo[1,2-f]phenanthridines via Pd-catalyzed intramolecular direct C(sp(2))-H arylation. The one-pot tandem approaches to the polycyclic indole derivatives were also successfully achieved. PMID:25211172

  19. Energy efficient one-pot synthesis of durable superhydrophobic coating through nylon micro-rods

    NASA Astrophysics Data System (ADS)

    Simovich, T.; Wu, A. H.; Lamb, R. N.

    2014-03-01

    A durable and superhydrophobic coating was fabricated at room temperature through encapsulating nylon micro-rods in a hydrophobic silica shell. This was achieved through the precipitation of miniemulsified nylon under high shear to generate micro-rods with high aspect ratio in the presence of methyltrimethoxysilane. The resultant coating structure resembles a network of highly entangled micro-rods that give rise to both surface roughness and hydrophobicity, resulting in contact angles greater than 155°. The embedded nylon polymer within the micro-rods imparts significant mechanical durability to the surface, resulting in a coating hardness of 2H using the pencil hardness test.

  20. A one-pot synthesis of 1,6,9,13-tetraoxadispiro(4.2.4.2)tetradecane by hydrodeoxygenation of xylose using a palladium catalyst

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In an effort to expand the number of biobased chemicals available from sugars, xylose has been converted to 1,6,9,13-tetraoxadispiro(4.2.4.2)tetradecane in a one-pot reaction using palladium supported on silica-alumina as the catalyst. The title compound is produced in 35-40% yield under 7 MPa H2 pr...

  1. Consecutive condensation, C-N and N-N bond formations: a copper- catalyzed one-pot three-component synthesis of 2H-indazole.

    PubMed

    Kumar, Manian Rajesh; Park, Ahbyeol; Park, Namjin; Lee, Sunwoo

    2011-07-01

    2H-Indazoles are synthesized using copper-catalyzed, one-pot, three-component reactions of 2-bromobenzaldehydes, primary amines, and sodium azide. A copper catalyst plays the key role in the formation of C-N and N-N bonds. This method has a broad substrate scope with a high tolerance for a variety of functional groups. PMID:21644532

  2. One-Pot Synthesis of Multifunctional Polymers by Light-Controlled Radical Polymerization and Enzymatic Catalysis with Candida antarctica Lipase B.

    PubMed

    Hrsic, Emin; Keul, Helmut; Möller, Martin

    2015-12-01

    The preparation of multifunctional polymers and block copolymers by a straightforward one-pot reaction process that combines enzymatic transacylation with light-controlled polymerization is described. Functional methacrylate monomers are synthesized by enzymatic transacylation and used in situ for light-controlled polymerization, leading to multifunctional methacrylate-based polymers with well-defined microstructure.

  3. One-pot synthesis of hierarchical Cu{sub 2}O/Cu hollow microspheres with enhanced visible-light photocatalytic activity

    SciTech Connect

    Hong, Tianjie; Tao, Feifei Lin, Jiudong; Ding, Wei; Lan, Mingxuan

    2015-08-15

    The hierarchical Cu{sub 2}O/Cu hollow microspheres have been fabricated by the one-pot solvothermal redox method, which is one-step approach without any surfactant and template. By using the HRTEM, XRD, XPS and UV–vis spectroscopy, the as-prepared product is composed of Cu{sub 2}O and Cu with energy band gap of 1.72 eV. Based on the time-dependent experiments, the content of Cu{sub 2}O and Cu compositions can be effectively controlled by adjusting the reaction time and a possible mechanism is proposed. In addition, using various dye molecules to stimulate pollutants, the hierarchical Cu{sub 2}O/Cu hollow microspheres reacted for 8 h exhibit excellent visible-light photocatalytic activities, which is much higher than those of the Cu{sub 2}O/Cu catalysts formed at the shorter reaction time, commercial Cu{sub 2}O powder and the mixture of alone Cu{sub 2}O and Cu. This enhanced photocatalytic performance makes these hierarchical Cu{sub 2}O/Cu hollow microspheres a kind of efficient visible-light photocatalyst in removing some organic compounds in wastewater. - Graphical abstract: The hierarchical Cu{sub 2}O/Cu hollow microspheres with adjustable components have been synthesized by one-step solvothermal redox approach. The special structures and composition lead to the excellent visible-light photocatalytic activity. - Highlights: • The hierarchical Cu{sub 2}O/Cu hollow microspheres are fabricated by one-step approach. • The content of Cu{sub 2}O and Cu can be controlled by adjusting the reaction time. • The material exhibits a better visible-light photocatalytic activity and stability. • Degradation kinetics of MO by Cu{sub 2}O/Cu fits the pseudo first-order model.

  4. Melamine-assisted one-pot synthesis of hierarchical nitrogen-doped carbon@MoS₂ nanowalled core-shell microspheres and their enhanced Li-storage performances.

    PubMed

    Sun, Fugen; Wei, Yanju; Chen, Jianzhuang; Long, Donghui; Ling, Licheng; Li, Yongsheng; Shi, Jianlin

    2015-08-14

    A facile and scalable one-pot approach has been developed to synthesize carbon@MoS2 core-shell microspheres by a hydrothermal method, which involves the fast formation of melamine-resorcinol-formaldehyde polymeric microspheres in situ, followed by direct growth of the MoS2 nanowalls on them. The results give unequivocal proof that melamine could be the key to forming the core-shell microspherical morphology, and the contents of MoS2 shells can be easily tuned by initial ratios of the precursors. After a simple heat treatment, the obtained carbon@MoS2 microspheres simultaneously integrate the nitrogen-doped carbon cores and the hierarchical shells which consist of few-layered MoS2 nanowalls with an expanded interlayer spacing. Their unique architectures are favourable for high electronic/ionic conductivity and accommodate volume strain during the electrochemical reaction of the MoS2 anodes in lithium-ion batteries. Thus, a very high reversibility capacity of 771 mA h g(-1) at 100 mA g(-1) after 100 cycles, and a rate capacity of 598 mA h g(-1) at 2000 mA g(-1) could be achieved for the carbon@MoS2 core-shell microspheres with the optimal composition. Furthermore, a thin carbon coating on the carbon@MoS2 microspheres could further increase the reversible capacity to 856 mA h g(-1) after 100 cycles at 100 mA g(-1). These encouraging results suggest that such a facile and efficient protocol can provide a new pathway to produce hierarchical core-shell microspheres which integrate the structural, morphological and compositional design rationales for advanced lithium-ion batteries.

  5. One-Pot Low Temperature Synthesis and Characterization Studies of Nanocrystalline α-Fe2O3 Based Dye Sensitized Solar Cells.

    PubMed

    Manikandan, A; Saravanan, A; Antony, S Arul; Bououdina, M

    2015-06-01

    Dye-sensitized solar cell (DSSC) based α-Fe2O3 nanostructures with two different morphologies, such as nanorods (FeONRs) and nanoparticles (FeONPs), were synthesized by one-pot low temperature method. The crystal structure and phase purity of the as-prepared samples were characterized by X-ray powder diffraction (XRD) and further determined by Rietveld refinements XRD analysis. The average crystallite size was calculated using Debye Sherrer formula, and it shows the range of 9.43-26.56 nm. The morphologies of the products were studied by high resolution scanning electron microscopy (HR-SEM) and it was confirmed by high resolution transmission electron microscopy (HR-TEM). The formation of pure α-Fe2O3 samples was further confirmed by energy dispersive X-ray (EDX) analysis. The optical properties and the band gap energy (E(g)) were measured by UV-Visible diffuse reflectance spectra (DRS) and photoluminescence (PL) spectra. The band gap energy was measured using Kubelka-Munk method, and the values are decreased from 2.36 eV to 2.21 eV as the temperature increased from 300 to 400 degrees C with increasing the crystallite size. Magnetic hysteresis (M-H) loop revealed that the as-prepared α-Fe2O3 samples displayed ferromagnetic behavior. FeONRs sample shows higher saturation magnetization (M(s)) value (40.21 emu/g) than FeONPs sample (23.06 emu/g). The dye-sensitized solar cell based on the optimized FeONRs array reaches a conversion efficiency of 0.43%, which is higher than that obtained from FeONPs (0.29%) under the light radiation of 1000 W/m2.

  6. An efficient one-pot procedure for asymmetric bifunctionalization of 5,15-disubstituted porphyrins: a simple preparation of meso acyl-, alkoxycarbonyl-, and carbamoyl-substituted meso-formylporphyrins.

    PubMed

    Takanami, Toshikatsu; Wakita, Atsushi; Matsumoto, Jun; Sekine, Sadashige; Suda, Kohji

    2009-01-01

    An efficient one-pot procedure which converts 5,15-disubstituted porphyrins into their corresponding meso acyl-, alkoxycarbonyl-, and carbamoyl-substituted meso-formylporphyrins has been developed, where the procedure involves a sequential S(N)Ar reaction of porphyrins with PyMe(2)SiCH(2)Li, followed by acylation or related reactions and oxidation.

  7. SbCl3-catalyzed one-pot synthesis of 4,4′-diaminotriarylmethanes under solvent-free conditions: Synthesis, characterization, and DFT studies

    PubMed Central

    2011-01-01

    Summary A simple, efficient, and mild procedure for a solvent-free one-step synthesis of various 4,4′-diaminotriarylmethane derivatives in the presence of antimony trichloride as catalyst is described. Triarylmethane derivatives were prepared in good to excellent yields and characterized by elemental analysis, FTIR, 1H and 13C NMR spectroscopic techniques. The structural and vibrational analysis were investigated by performing theoretical calculations at the HF and DFT levels of theory by standard 6-31G*, 6-31G*/B3LYP, and B3LYP/cc-pVDZ methods and good agreement was obtained between experimental and theoretical results. PMID:21445373

  8. A new Co(2)(CO8-mediated tandem [5 + 1]/[2 + 2 + 1]-cycloaddition reaction: a one-pot synthesis of tricyclic delta-lactones from cis-epoxy ene-ynes.

    PubMed

    Odedra, Arjan; Wu, Chang-Jung; Madhushaw, Reniguntala J; Wang, Su-Lein; Liu, Rai-Shung

    2003-08-13

    In the presence of Co2(CO)8 and CO, cis-epoxyalkynes bearing a tether olefin undergo a tandem [5 + 1]/[2 + 2 + 1]-cycloaddition to give tricyclic delta-lactones efficiently in a one-pot operation. The reaction mechanism is proposed to involve a cobalt-coordinated cyclic allene species.

  9. Elucidating the structure-property relationships of donor-π-acceptor dyes for dye-sensitized solar cells (DSSCs) through rapid library synthesis by a one-pot procedure.

    PubMed

    Fuse, Shinichiro; Sugiyama, Sakae; Maitani, Masato M; Wada, Yuji; Ogomi, Yuhei; Hayase, Shuzi; Katoh, Ryuzi; Kaiho, Tatsuo; Takahashi, Takashi

    2014-08-18

    The creation of organic dyes with excellent high power conversion efficiency (PCE) is important for the further improvement of dye-sensitized solar cells. We wish to describe the rapid synthesis of a 112-membered donor-π-acceptor dye library by a one-pot procedure, evaluation of PCEs, and elucidation of structure-property relationships. No obvious correlations between ε, and the η were observed, whereas the HOMO and LUMO levels of the dyes were critical for η. The dyes with a more positive E(HOMO), and with an E(LUMO)<-0.80 V, exerted higher PCEs. The proper driving forces were crucial for a high J(sc), and it was the most important parameter for a high η. The above criteria of E(HOMO) and E(LUMO) should be useful for creating high PCE dyes; nevertheless, that was not sufficient for identifying the best combination of donor, π, and acceptor blocks. Combinatorial synthesis and evaluation was important for identifying the best dye.

  10. Microwave-assisted One-pot Synthesis of N-succinimidyl-4-[18F]fluorobenzoate ([18F]SFB)

    PubMed Central

    Lin, Wei-Yu; Wang, Ming-wei; Liu, Kan; Shen, Clifton Kwang-Fu

    2011-01-01

    beneficial for its adaption to an automated process. Herein, we report a concise preparation of [18F]SFB, based on a simplified one-pot microwave-assisted synthesis (Figure 1). Our approach does not require purification between steps or any aqueous reagents. In addition, microwave irradiation, which has been used in the syntheses of several PET tracers,38-41 can gives higher RCYs and better selectivity than the corresponding thermal reactions or they provide similar yields in shorter reaction times.38 Most importantly, when labeling biomolecules, the time saved could be diverted to subsequent bioconjugation or PET imaging step.28,43 The novelty of our improved [18F]SFB synthesis is two-fold: (1) the anhydrous deprotection strategy requires no purification of intermediate(s) between each step and (2) the microwave-assisted radiochemical transformations enable the rapid, reliable production of [18F]SFB. PMID:21730951

  11. Shape dependent catalytic activity of nanoflowers and nanospheres of Pd4S generated via one pot synthesis and grafted on graphene oxide for Suzuki coupling.

    PubMed

    Singh, Ved Vati; Kumar, Umesh; Tripathi, Sandeep Nath; Singh, Ajai Kumar

    2014-09-01

    Nanoflowers and nanospheres of Pd4S have been prepared for the first time from a single source precursor complex, [PdCl2(PhS-CH2CH2CH2-NH2)] (), by its one pot thermolysis at 195 °C. In oleylamine, flower shaped nanoparticles of Pd4S were formed but in an oleic acid (OA) and octadecene (ODE) mixture (1 : 1) the product was nanospheres of Pd4S (size in the range ∼23-38 nm and 15-28 nm, respectively). These nanoparticles (NPs) were grafted on graphene oxide (GO) at room temperature to prepare nanocomposites, GO-Pd4S. HRTEM, powder X-ray diffraction (PXRD) and TEM-EDX have been used to authenticate the nanoparticles and their composites. XPS of Pd4S NPs indicates the oxidation states of Pd and S are both zero with a Pd : S ratio ∼4.1 : 0.9. For the catalysis of Suzuki-Miyaura coupling reactions the nanoparticles individually and in the form of composites with GO were explored. The flower shaped NPs are superior than the spherical ones for this catalysis in aqueous ethanol and the catalytic efficiency increases on grafting the nanoflowers/spheres onto GO. The conversion was ∼99% (in 5 h; at 80 °C) for the composite of graphene oxide (GO) with the Pd4S nanoflowers (Pd: 0.2 mol%). The catalytic efficiency follows the order GO-Pd4S-nanoflowers > GO-Pd4S-nanospheres > Pd4S nanoflowers > Pd4S nanospheres. The recyclability of the GO-Pd4S nanoflower catalyst was examined for the coupling reaction and conversion was found to be ∼46% in the fourth run even after increasing the reaction time to 12 h. To understand whether the catalytic process with the GO-Pd4S nanoflowers was homogeneous or heterogeneous mercury poisoning, triphenylphosphine and three phase tests were carried out. They suggest that active Pd leached from GO-Pd4S nanoflowers does the catalysis significantly in a homogeneous fashion. Overall the catalysis appears to be a cocktail of homogeneous and some heterogeneous nature.

  12. One-Pot Synthesis of Organic-Sulfur-Zinc Hybrid Materials via Polycondensation of a Zinc Salt and Thiols Generated in Situ from Cyclic Dithiocarbonates.

    PubMed

    Ochiai, Bungo; Konta, Hirohisa

    2015-08-17

    Soluble organic-sulfur-zinc hybrid polymers were prepared via a one-pot reaction consisting of ring-opening addition and subsequent polycondensation. The first reaction is the nucleophilic ring-opening addition of 2-ethylhexylamine to multifunctional cyclic dithiocarbonates giving multiple thiols in situ. The sequential polycondensation of the in situ generated thiols with Zn(OAc)2 gave the target hybrid polymers. This one-pot method enabled the use of a shorter amine than the previous polycondensation of Zn(OAc)2 and purified thiols, which required octadecylamine to obtain a soluble product. The obtained hybrid polymers may be cast as composite films with polystyrene and poly(methyl methacrylate). Owing to the shorter alkyl chain, the calculated nD values of the products (1.60 or 1.61) are higher than that of the previous product bearing octadecyl chains (1.53).

  13. One-Pot Synthesis of (NiFe2O4)x-(SrFe12O19)1-x Nanocomposites and Their Microwave Absorption Properties.

    PubMed

    Hazra, Subhenjit; Ghosh, Barun Kumar; Patra, Manoj Kumar; Jani, Raj Kumar; Vadera, Sampat Raj; Ghosh, Narendra Nath

    2015-09-01

    In this paper, we report a simple but novel aqueous solution based 'one-pot' method for preparation of (NiFe2O4)x-(SrFe12O19)1-x nanocomposites consist of hard ferrite-soft ferrite phases. A physical mixing method has also been employed to prepare nanocomposites having same compositions. The effects of synthetic methodologies on the microstructures of the nanocomposites as well as their magnetic and microwave absorption properties have been evaluated. Crystal structures and microstructures of these composites have been investigated by using X-ray diffraction, transmission electron microscope and scanning electron microscope. In the nanocomposites, prepared by both methods, presence of nanocrystalline NiFe2O4 and SrFe12O19 phases was detected. However, nanocomposites, prepared by one-pot method, possessed better homogeneous distribution of hard and soft ferrite phases than the nanocomposites, prepared by physical mixing method. Nanocomposites, prepared by one-pot method, demonstrated significant spring exchange coupling interaction between hard and soft ferrite phases and exhibited magnetically single phase behaviour. The spring exchange coupling interaction enhanced the magnetic properties (high saturation magnetization and coercivity) and microwave absorption properties of the nanocomposites, prepared by one-pot method, in comparison with the nanocomposites prepared by physical mixing method as well as pure NiFe2O4 and SrFe12O19 nanoparticles. Minimum reflection loss of the composite was ~ -17 dB (i.e., 98% absorption) at 8.2 GHz for an absorber thickness of 3.2 mm.

  14. One pot Click chemistry: A three component reaction for the synthesis of 2-mercaptobenzimidazole linked coumarinyl triazoles as anti-tubercular agents.

    PubMed

    Anand, Ashish; Kulkarni, Manohar V; Joshi, Shrinivas D; Dixit, Sheshagiri R

    2016-10-01

    2-Propargylthiobenzimidazole 1, 4-bromomethyl coumarins/1-aza-coumarins 2/3 and sodium azide have been reacted in one pot under Click chemistry conditions to give exclusively 1,4-disubstituted triazoles 5a-n. Anti-tubercular assays against M. tuberculosis (H37Rv) coupled with in silico molecular docking studies indicated that dimethyl substituents 5c and 5d showed promising activity with higher C-score values. PMID:27595420

  15. Lewis acid-promoted reactions of zirconacyclopentadienes with isocyanates. A one-pot three-component synthesis of multiply-substituted iminocyclopentadienes from one isocyanate and two alkynes.

    PubMed

    Lu, Jiang; Mao, Guoliang; Zhang, Wenxiong; Xi, Zhenfeng

    2005-10-14

    Multiply-substituted iminocyclopentadienes were formed from Lewis acid-promoted reactions of zirconacyclopentadienes and isocyanates via a one-pot three-component coupling process; the C=O double bond of the RN=C=O moiety in the isocyanate was cleaved, and the isocyanates behaved formally as a one-carbon unit with Lewis acid-dependent and substituent-dependent reactions being realized.

  16. One-Pot Synthesis of (NiFe2O4)x-(SrFe12O19)1-x Nanocomposites and Their Microwave Absorption Properties.

    PubMed

    Hazra, Subhenjit; Ghosh, Barun Kumar; Patra, Manoj Kumar; Jani, Raj Kumar; Vadera, Sampat Raj; Ghosh, Narendra Nath

    2015-09-01

    In this paper, we report a simple but novel aqueous solution based 'one-pot' method for preparation of (NiFe2O4)x-(SrFe12O19)1-x nanocomposites consist of hard ferrite-soft ferrite phases. A physical mixing method has also been employed to prepare nanocomposites having same compositions. The effects of synthetic methodologies on the microstructures of the nanocomposites as well as their magnetic and microwave absorption properties have been evaluated. Crystal structures and microstructures of these composites have been investigated by using X-ray diffraction, transmission electron microscope and scanning electron microscope. In the nanocomposites, prepared by both methods, presence of nanocrystalline NiFe2O4 and SrFe12O19 phases was detected. However, nanocomposites, prepared by one-pot method, possessed better homogeneous distribution of hard and soft ferrite phases than the nanocomposites, prepared by physical mixing method. Nanocomposites, prepared by one-pot method, demonstrated significant spring exchange coupling interaction between hard and soft ferrite phases and exhibited magnetically single phase behaviour. The spring exchange coupling interaction enhanced the magnetic properties (high saturation magnetization and coercivity) and microwave absorption properties of the nanocomposites, prepared by one-pot method, in comparison with the nanocomposites prepared by physical mixing method as well as pure NiFe2O4 and SrFe12O19 nanoparticles. Minimum reflection loss of the composite was ~ -17 dB (i.e., 98% absorption) at 8.2 GHz for an absorber thickness of 3.2 mm. PMID:26716212

  17. One pot Click chemistry: A three component reaction for the synthesis of 2-mercaptobenzimidazole linked coumarinyl triazoles as anti-tubercular agents.

    PubMed

    Anand, Ashish; Kulkarni, Manohar V; Joshi, Shrinivas D; Dixit, Sheshagiri R

    2016-10-01

    2-Propargylthiobenzimidazole 1, 4-bromomethyl coumarins/1-aza-coumarins 2/3 and sodium azide have been reacted in one pot under Click chemistry conditions to give exclusively 1,4-disubstituted triazoles 5a-n. Anti-tubercular assays against M. tuberculosis (H37Rv) coupled with in silico molecular docking studies indicated that dimethyl substituents 5c and 5d showed promising activity with higher C-score values.

  18. Fe3O4@SiO2-NH2 Nanocomposite as a Robust and Effective Catalyst for the One-pot Synthesis of Polysubstituted Dihydropyridines.

    PubMed

    Ghasemzadeh, Mohammad Ali; Abdollahi-Basir, Mohammad Hossein

    2016-01-01

    A practical, simple and efficient method for the synthesis of polysubstituted dihydropyridines was described via multicomponent reactions of aldehydes, arylamines, dimethyl acetylenedicarboxylate and malononitrile/ethyl acetoacetate in the presence of Fe3O4@SiO2-NH2 nanocomposites. The present methodology provides a novel and efficient method for the synthesis of dihydropyridine derivatives with some advantages, such as excellent yields, short reaction times, recoverability and low catalyst loading. The nanomagnetic catalyst could be readily recovered using an external magnet and reused several times without any significant loss in activity. The catalyst was fully characterized by FT-IR, SEM, XRD, EDX and VSM analysis. PMID:27640390

  19. Cu-Catalyzed Multicomponent Reaction of Styrenes, Perfluoroalkyl Halide, Alcohol, and tert-Butyl Hydroperoxide: One-Pot Synthesis of (Z)-β-Alkoxyperfluoroalkenone.

    PubMed

    Luo, Qiang; Liu, Chunmei; Tong, Jingjing; Shao, Ying; Shan, Wenyu; Wang, Hanghang; Zheng, Hao; Cheng, Jiang; Wan, Xiaobing

    2016-04-15

    An efficient synthesis of Z-perfluoroalkyl-substituted enones by a multicomponent reaction strategy has been described. A variety of elusive perfluoroalkylated enones are furnished under mild reaction conditions in good yields with unique chemo- and stereoselectivity. A sequence of radical-mediated Kornblum-DeLaMare reaction, Michael addition, and HF elimination is proposed for the mechanism. PMID:26980724

  20. One-pot green synthesis of oxygen-rich nitrogen-doped graphene quantum dots and their potential application in pH-sensitive photoluminescence and detection of mercury(II) ions.

    PubMed

    Shi, Bingfang; Zhang, Liangliang; Lan, Chuanqing; Zhao, Jingjin; Su, Yubin; Zhao, Shulin

    2015-09-01

    Nitrogen doping has been a powerful method to modulate the properties of carbon materials for various applications, and N-doped graphene quantum dots (GQDs) have gained remarkable interest because of their unique chemical, electronic, and optical properties. Herein, we introduce a facile one-pot solid-phase synthesis strategy for N-doped GQDs using citric acid (CA) as the carbon source and 3,4-dihydroxy-L-phenylalanine (L-DOPA) as the N source. The as-prepared N-GQDs with oxygen-rich functional groups are uniform with an average diameter of 12.5 nm. Because of the introduction of nitrogen atoms, N-GQDs exhibit excitation-wavelength-independent fluorescence with the maximum emission at 445 nm, and a high quantum yield of 18% is achieved at an excitation wavelength of 346 nm. Furthermore, a highly efficient fluorosensor based on the as-prepared N-GQDs was developed for the detection of Hg(2+) because of the effective quenching effect of metal ions via nonradiative electron transfer. This fluorosensor exhibits high sensitivity toward Hg(2+) with a detection limit of 8.6 nM. The selectivity experiments reveal that the fluorescent sensor is specific for Hg(2+). Most importantly, the practical use of the sensor based on N-GQDs for Hg(2+) detection was successfully demonstrated in river-water samples. PMID:26003702

  1. One-pot green synthesis of oxygen-rich nitrogen-doped graphene quantum dots and their potential application in pH-sensitive photoluminescence and detection of mercury(II) ions.

    PubMed

    Shi, Bingfang; Zhang, Liangliang; Lan, Chuanqing; Zhao, Jingjin; Su, Yubin; Zhao, Shulin

    2015-09-01

    Nitrogen doping has been a powerful method to modulate the properties of carbon materials for various applications, and N-doped graphene quantum dots (GQDs) have gained remarkable interest because of their unique chemical, electronic, and optical properties. Herein, we introduce a facile one-pot solid-phase synthesis strategy for N-doped GQDs using citric acid (CA) as the carbon source and 3,4-dihydroxy-L-phenylalanine (L-DOPA) as the N source. The as-prepared N-GQDs with oxygen-rich functional groups are uniform with an average diameter of 12.5 nm. Because of the introduction of nitrogen atoms, N-GQDs exhibit excitation-wavelength-independent fluorescence with the maximum emission at 445 nm, and a high quantum yield of 18% is achieved at an excitation wavelength of 346 nm. Furthermore, a highly efficient fluorosensor based on the as-prepared N-GQDs was developed for the detection of Hg(2+) because of the effective quenching effect of metal ions via nonradiative electron transfer. This fluorosensor exhibits high sensitivity toward Hg(2+) with a detection limit of 8.6 nM. The selectivity experiments reveal that the fluorescent sensor is specific for Hg(2+). Most importantly, the practical use of the sensor based on N-GQDs for Hg(2+) detection was successfully demonstrated in river-water samples.

  2. A facile one-pot hydrothermal synthesis of β-MnO{sub 2} nanopincers and their catalytic degradation of methylene blue

    SciTech Connect

    Cheng, Gao; Yu, Lin Lin, Ting; Yang, Runnong; Sun, Ming; Lan, Bang; Yang, Lili; Deng, Fangze

    2014-09-15

    Branched β-MnO{sub 2} bipods with novel nanopincer morphology were prepared by a facile one-pot hydrothermal method via a redox reaction between NaClO{sub 3} and MnSO{sub 4} in sulfuric acid solution without using any surfactants or templates. The products were characterized in detail by various techniques including X-ray powder diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, surface area analyzer, field emission scanning electron microscopy and transmission electron microscopy. Results show that the obtained β-MnO{sub 2} nanopincers consist of two sharp nanorods with a diameter of 100–200 nm and a length of 1–2 μm. The concentration of H{sub 2}SO{sub 4} solution plays an important role in controlling the crystal phase and morphology of the final product. A possible formation mechanism for the β-MnO{sub 2} nanopincers was proposed. Moreover, these β-MnO{sub 2} nanostructures exhibited better catalytic performance than the commercial MnO{sub 2} particles to decompose methyl blue (MB) in the presence of H{sub 2}O{sub 2}. - Graphical abstract: Branched β-MnO{sub 2} bipods with novel nanopincer morphology were prepared by a facile one-pot hydrothermal method through oxidizing MnSO{sub 4} with NaClO{sub 3} in H2SO{sub 4} condition without using any surfactants or templates. - Highlights: {sup •} Branched β-MnO{sub 2} nanopincers were prepared by a facile one-pot hydrothermal method. {sup •} Morphology and crystal phase of MnO{sub 2} were controlled by the H{sub 2}SO{sub 4} concentration. {sup •} A possible formation mechanism for the obtained β-MnO{sub 2} nanopincers was proposed. {sup •} The products showed great catalytic performance in degradation of methylene blue.

  3. One-pot synthesis of 4'-alkyl-4-cyanobiaryls on the basis of the terephthalonitrile dianion and neutral aromatic nitrile cross-coupling.

    PubMed

    Peshkov, Roman Yu; Panteleeva, Elena V; Chunyan, Wang; Tretyakov, Evgeny V; Shteingarts, Vitalij D

    2016-01-01

    A convenient one-pot approach to alkylcyanobiaryls is described. The method is based on biaryl cross-coupling between the sodium salt of the terephthalonitrile dianion and a neutral aromatic nitrile in liquid ammonia, and successive alkylation of the long-lived anionic intermediate with alkyl bromides. The reaction is compatible with benzonitriles that contain methyl, methoxy and phenyl groups, fluorine atoms, and a 1-cyanonaphthalene residue. The variety of ω-substituted alkyl bromides, including an extra bromine atom, a double bond, cyano and ester groups, as well as a 1,3-dioxane fragment are suitable as alkylation reagents. PMID:27559409

  4. One-pot synthesis of single-crystal Pt nanoplates uniformly deposited on reduced graphene oxide, and their high activity and stability on the electrocalalytic oxidation of methanol.

    PubMed

    Hao, Yanfei; Wang, Xudan; Shen, Jianfeng; Yuan, Junhua; Wang, Ai-Jun; Niu, Li; Huang, Shengtang

    2016-04-01

    We demonstrate a one-pot thermoreduction approach towards the preparation of single-crystal Pt nanoplates, which were uniformly deposited on the reduced graphene oxide (RGO) using polyvinylpyrrolidone (PVP) as a stabilizer. The size of Pt nanoplates can be tuned from 6.8 to 10.1 nm by controlling Pt loading. The as-prepared Pt/PVP/RGO catalysts show high stability and activity towards the methanol oxidation reaction (MOR). Their MOR current can reach up to 401 mA mg(-1) Pt and MOR current can maintain 89.4% of its initial value after 10 000 potential cycles.

  5. One-pot synthesis of 4′-alkyl-4-cyanobiaryls on the basis of the terephthalonitrile dianion and neutral aromatic nitrile cross-coupling

    PubMed Central

    Peshkov, Roman Yu; Chunyan, Wang; Tretyakov, Evgeny V; Shteingarts, Vitalij D

    2016-01-01

    Summary A convenient one-pot approach to alkylcyanobiaryls is described. The method is based on biaryl cross-coupling between the sodium salt of the terephthalonitrile dianion and a neutral aromatic nitrile in liquid ammonia, and successive alkylation of the long-lived anionic intermediate with alkyl bromides. The reaction is compatible with benzonitriles that contain methyl, methoxy and phenyl groups, fluorine atoms, and a 1-cyanonaphthalene residue. The variety of ω-substituted alkyl bromides, including an extra bromine atom, a double bond, cyano and ester groups, as well as a 1,3-dioxane fragment are suitable as alkylation reagents. PMID:27559409

  6. One-pot synthesis of monodisperse palladium-copper nanocrystals supported on reduced graphene oxide nanosheets with improved catalytic activity and methanol tolerance for oxygen reduction reaction

    NASA Astrophysics Data System (ADS)

    Lv, Jing-Jing; Li, Shan-Shan; Wang, Ai-Jun; Mei, Li-Ping; Feng, Jiu-Ju; Chen, Jian-Rong; Chen, Zhaojiang

    2014-12-01

    Monodisperse bimetallic alloyed palladium-copper nanocrystals are uniformly supported on reduced graphene oxide nanosheets by a one-pot solvothermal strategy, with an average size of 6.81 nm. As a result, the as-prepared nanocomposites have the enlarged electrochemically active surface area (49.2 m2 g-1), and display the improved electrocatalytic performance and high methanol-tolerance ability for oxygen reduction reaction in alkaline media, compared with commercial Pd black and RGOs. Those RGOs-supporting Pd-Cu alloys would have potential applications in fuel cells.

  7. One-pot synthesis of 2,5-dihydropyrroles from terminal alkynes, azides, and propargylic alcohols by relay actions of copper, rhodium, and gold.

    PubMed

    Miura, Tomoya; Tanaka, Takamasa; Matsumoto, Kohei; Murakami, Masahiro

    2014-12-01

    Relay actions of copper, rhodium, and gold formulate a one-pot multistep pathway, which directly gives 2,5-dihydropyrroles starting from terminal alkynes, sulfonyl azides, and propargylic alcohols. Initially, copper-catalyzed 1,3-dipolar cycloaddition of terminal alkynes with sulfonyl azides affords 1-sulfonyl-1,2,3-triazoles, which then react with propargylic alcohols under the catalysis of rhodium. The resulting alkenyl propargyl ethers subsequently undergo the thermal Claisen rearrangement to give α-allenyl-α-amino ketones. Finally, a gold catalyst prompts 5-endo cyclization to produce 2,5-dihydropyrroles. PMID:25345587

  8. Facile one-pot synthesis of carbon/calcium phosphate/Fe3O4 composite nanoparticles for simultaneous imaging and pH/NIR-responsive drug delivery.

    PubMed

    Gou, Mingyu; Li, Shengnan; Zhang, Lingyu; Li, Lu; Wang, Chungang; Su, Zhongmin

    2016-09-25

    A facile one-pot synthetic strategy was explored to synthesize carbon/calcium phosphate/Fe3O4 composite nanoparticles (carbon/CaP/Fe3O4 composite NPs). Taking advantage of the unique structure including mesoporous, small CaP and Fe3O4 subunits homogeneously distributed in a carbon matrix, carbon/CaP/Fe3O4 NPs integrate high drug loading, pH/NIR-sensitive, photothermal and magnetic properties into one nanoplatform for cancer theranostics.

  9. Mechanochemical solid-state synthesis of 2-aminothiazoles, quinoxalines and benzoylbenzofurans from ketones by one-pot sequential acid- and base-mediated reactions.

    PubMed

    Nagarajaiah, Honnappa; Mishra, Abhaya Kumar; Moorthy, Jarugu Narasimha

    2016-04-26

    α-Chloroketones - obtained by the atom-economical chlorination of ketones with trichloroisocyanuric acid (TCCA) in the presence of p-TSA under ball-milling conditions - were set up for a sequential base-mediated condensation reaction with thiourea/thiosemicarbazides, o-phenylenediamine and salicylaldehyde to afford 2-aminothiazoles, 2-hydrazinylthiazoles, quinoxalines and benzoylbenzofurans, respectively, in respectable yields. The viability of one-pot sequential acid- and base-mediated reactions in the solid state under ball-milling conditions is thus demonstrated.

  10. Traceless OH-Directed Wacker Oxidation-Elimination, an Alternative to Wittig Olefination/Aldol Condensation: One-Pot Synthesis of α,β-Unsaturated and Nonconjugated Ketones from Homoallyl Alcohols.

    PubMed

    Bethi, Venkati; Fernandes, Rodney A

    2016-09-16

    A new method for one-pot synthesis of β-substituted and β,β-disubstituted α,β-unsaturated methyl ketones from homoallyl alcohols by sequential PdCl2/CrO3-promoted Wacker process followed by an acid-mediated dehydration reaction has been developed. Remarkably, internal homoallyl alcohols delivered regioselectively nonconjugated unsaturated carbonyl compounds under the same protocol. A new starting material-based synthesis of α,β-unsaturated and nonconjugated methyl ketones is demonstrated. PMID:27562136

  11. Facile synthesis of core-shell/hollow anisotropic particles via control of cross-linking during one-pot dispersion polymerization.

    PubMed

    Liu, Yanan; Ma, Yuhong; Liu, Lianying; Yang, Wantai

    2015-05-01

    Preparation of anisotropic particles based on seed phase separation involves multiple processes, and asymmetrical structures and surfaces cannot be produced when anisotropic shapes emerge. In conventional one-pot dispersion polymerization (Dis.P) using cross-linker, only spherical particles are prepared due to rapid and high cross-linking. Herein, monodisperse snowman-like particles with core-shell/hollow structures and partially rough surface were synthesized straightforward by a modified one-pot Dis.P, in which ethylene glycol and water (6/4, vol.) were used as medium, and ammonium persulfate (APS) aqueous solution, vinyl acetate (VA) and/or acrylic acid (AA), divinylbenzene (DVB) and styrene (St) were added at 6h. The cross-linking of growing particles was confined to exterior (forming cross-linked shell), and gel contents were low, leading to phase separation. Asymmetrical morphologies, structures, sizes and surface roughness were flexibly tuned by varying amounts of APS, VA and/or AA, water and DVB, and DVB adding speed. At low APS contents or high DVB amounts, the inhomogeneous cross-linking of head enabled its phase to separate, producing elongated head. With addition of VA and AA, phase separations inside head and body were induced, generating hollow structure. Adding DVB very slowly, nonlinear growth of third compartment occurred, forming bowed head. PMID:25626132

  12. A facile one-pot method to synthesize a three-dimensional graphene@carbon nanotube composite as a high-efficiency microwave absorber.

    PubMed

    Wang, Lei; Huang, Ying; Li, Chao; Chen, Junjiao; Sun, Xu

    2015-01-21

    A novel three-dimensional graphene@carbon nanotube (CNTs) composite has been prepared using a facile one-pot pyrolysis strategy using urea as the carbon source, in which the density and length of CNTs on graphene are rationally tuned by adding an appropriate amount of urea to a precursor mixture. Correspondingly, the density and length of CNTs on graphene have a significant effect on the microwave absorption properties of graphene@CNTs. When most of the graphene surface is clearly covered by the CNTs whose length ranges from 300 to 600 nm, the graphene@CNT composite exhibits excellent microwave absorption properties. The maximum reflection loss value can reach -44.6 dB at 8.6 GHz and the absorption bandwidth with a reflection loss below -10 dB ranges from 7.1 to 10.4 GHz with an addition amount of only 5 wt% graphene@CNTs composite in the paraffin matrix.

  13. One-Pot Fabrication of Mesoporous Core-Shell Au@PtNi Ternary Metallic Nanoparticles and Their Enhanced Efficiency for Oxygen Reduction Reaction.

    PubMed

    Shi, Qiurong; Zhu, Chengzhou; Fu, Shaofang; Du, Dan; Lin, Yuehe

    2016-02-01

    Currently, Pt-based nanomaterials with tailorable shapes, structures, and morphologies are the most popular electrocatalysts for oxygen reduction reaction, which is a significant cathode reaction in fuel cells for renewable energy applications. We have successfully synthesized mesoporous core-shell Au@PtNi ternary metallic nanoparticles through a one-pot reduction method for cathodic materials used as oxygen reduction reaction catalysts. The as-synthesized nanoparticles exhibited superior catalytic activities and long-term stabilities compared with mesoporous core-shell Au@Pt nanoparticles and commercial Pt/C. The unique mesoporous core-shell structures as well as the alloy shells enable the enhanced electrochemical oxygen reduction reaction performances of the Pt-based materials via the electronic effect and geometric effect, holding great promise in fuel cell application.

  14. One-pot synthesis, structural characterization, UV-Vis and electrochemical analyses of new Schiff base complexes of Fe(III), Ni(II) and Cu(II)

    NASA Astrophysics Data System (ADS)

    Back, Davi Fernando; de Oliveira, Gelson Manzoni; Fontana, Liniquer Andre; Ramão, Brenda Fiorin; Roman, Daiane; Iglesias, Bernardo Almeida

    2015-11-01

    The complexes [Ni(Pyr2tetam-2H)]·2H2O (1) (Pyr2tetam = (pyridoxyl)2-N1,N4-triethylenetetramine), [Fe(Pyr2tetam-2H)](ClO4)·H2O (2) and [Cu(Pyrtetam-H)](ClO4) (3) (Pyrtetam = pyridoxyl-N1-triethylenetetramine) were obtained through one pot reactions of triethylenetetramine, pyridoxal chloridrate, triethylamine and the metal salts Ni(ClO4)2·6H2O, Fe(ClO4)2·6H2O and Cu(ClO4)2·6H2O. In complexes 1 and 2 the metal centers present a distorted octahedral coordination, while complex 3 shows a square pyramidal configuration. The structures were characterized through X-ray diffractometry, IR and UV-Vis spectra. Cyclic voltammograms of the title compounds are also presented and discussed.

  15. One-pot synthesis of porous Fe3O4 shell/silver core nanocomposites used as recyclable magnetic antibacterial agents

    NASA Astrophysics Data System (ADS)

    Fang, Weijun; Zheng, Jun; Chen, Cheng; Zhang, Huabing; Lu, Yunxia; Ma, Ling; Chen, Guangjun

    2014-05-01

    Porous Fe3O4 shell/silver core nanocomposites featuring sustainable and recyclable antibacterial activity have been successfully prepared via a facile one-pot hydrothermal method. The unique structural feature of the Ag@Fe3O4 nanocomposites with Ag embedded in porous Fe3O4 shell endows them with the ability of sustained-release of silver ions. Their antimicrobial activity studies were investigated on both Gram negative Escherichia coli and Gram positive Bacillus subtilis, which demonstrate that the nanocomposites are highly toxic to microorganisms and exhibit sustainable antibacterial activity. Besides, the Ag@Fe3O4 nanocomposites can be separated easily from the medium by a small magnet, which provided an effective way to eliminate the residual nanosilver from the surroundings. We finally demonstrate that the recovered nanocomposites exhibit recyclable antibacterial activity, acting as an ideal long-acting antibacterial agent.

  16. One-pot synthesis and biological evaluation of 2-pyrrolidinyl-4-amino-5-(3',4',5'-trimethoxybenzoyl)thiazole: a unique, highly active antimicrotubule agent.

    PubMed

    Romagnoli, Romeo; Baraldi, Pier Giovanni; Lopez Cara, Carlota; Kimatrai Salvador, Maria; Bortolozzi, Roberta; Basso, Giuseppe; Viola, Giampietro; Balzarini, Jan; Brancale, Andrea; Fu, Xian-Hua; Li, Jun; Zhang, Su-Zhan; Hamel, Ernest

    2011-12-01

    A wide variety of small molecules with diverse molecular scaffolds inhibit microtubule formation. In this article we report a one-pot procedure for the preparation of a novel 2-(N-pyrrolidinyl)-4-amino-5-(3',4',5'-trimethoxybenzoyl)thiazole in which the size of the substituent at the C-2 position of the thiazole ring plays an essential role in compound activity. The most active agent (3f) inhibited at submicromolar concentrations the growth of tumor cell lines. It also inhibited tubulin polymerization with an activity quantitatively similar to that of CA-4, and treatment of HeLa cells resulted in their arrest at the G2-M phase of the cell cycle. Furthermore, 3f was effective against multidrug resistant cancer cells and inhibited the growth of the HT-29 xenograft in a nude mouse model. This indicated that 3f is a promising new antimitotic agent with encouraging preclinical potential.

  17. Dielectric barrier discharge-assisted one-pot synthesis of carbon quantum dots as fluorescent probes for selective and sensitive detection of hydrogen peroxide and glucose.

    PubMed

    He, Duhong; Zheng, Chengbin; Wang, Qiang; He, Chunlin; Lee, Yong-Ill; Wu, Li; Hou, Xiandeng

    2015-09-01

    In this work, we proposed a dielectric barrier discharge (DBD)-assisted one-pot strategy to fabricate carbon quantum dots (CQDs) using only one reagent N, N-dimethylformamide (DMF) at atmospheric pressure and room temperature. The experimental conditions were carefully investigated, and the prepared CQDs were characterized by using UV-vis spectrophotometer, fluorescence spectrophotometer, Fourier transform infrared (FTIR) spectrometer, transmission electron microscopy (TEM) and X-ray photoelectron spectrometer (XPS). The CQDs have an average size of 3.6 nm in diameter with narrow size distribution, and can be used as highly selective and sensitive fluorescence probes for hydrogen peroxide and glucose, with limits of detection of 3.8 μM and 3.5 μM, respectively.

  18. One-pot enzymatic synthesis of docosahexaenoic acid-rich triacylglycerols at the sn-1(3) position using by-product from selective hydrolysis of tuna oil.

    PubMed

    Nagao, Toshihiro; Watanabe, Yomi; Maruyama, Kazuaki; Momokawa, Yuusuke; Kishimoto, Noriaki; Shimada, Yuji

    2011-01-31

    Docosahexaenoic acid (DHA)-rich oil has been industrially produced by selective hydrolysis of tuna oil with a lipase that acts weakly on DHA. The free fatty acids (FFAs) generated in this process as by-products contain a high DHA concentration (46wt%) but are treated as industrial waste. This study attempted to reuse these by-product FFAs using a one-pot process, and succeeded in producing triacylglycerols (TAGs) through the esterification of the by-product FFAs with glycerol using immobilized Rhizomucor miehei lipase. Regiospecific analysis of the resulting TAGs showed that the content of DHA at the sn-1(3) position (51.7mol%) was higher than the content of DHA at the sn-2 position (17.3mol%). The DHA distribution in TAGs synthesized in this study was similar to the DHA distribution in TAGs from seal oil.

  19. Nickel-Catalyzed Reductive Cross-Coupling of Benzyl Chlorides with Aryl Chlorides/Fluorides: A One-Pot Synthesis of Diarylmethanes.

    PubMed

    Zhang, Jie; Lu, Gusheng; Xu, Jin; Sun, Hongmei; Shen, Qi

    2016-06-17

    The first nickel-catalyzed, magnesium-mediated reductive cross-coupling between benzyl chlorides and aryl chlorides or fluorides is reported. A variety of diarylmethanes can be prepared in good to excellent yields in a one-pot manner using easy-to-access mixed PPh3/NHC Ni(II) complexes of Ni(PPh3)(NHC)Br2 (NHC = 1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene, IPr, 1a; 1,3-di-tert-butylimidazol-2-ylidene, ItBu, 1b) as catalyst precursors. Activation of polychloroarenes or chemoselective cross-coupling based on the difference in catalytic activity between 1a and 1b is used to construct oligo-diarylmethane motifs. PMID:27268781

  20. One-pot synthesis of highly greenish-yellow fluorescent nitrogen-doped graphene quantum dots for pyrophosphate sensing via competitive coordination with Eu(3+) ions.

    PubMed

    Lin, Liping; Song, Xinhong; Chen, Yiying; Rong, Mingcong; Zhao, Tingting; Jiang, Yaqi; Wang, Yiru; Chen, Xi

    2015-10-01

    Highly fluorescent nitrogen-doped graphene quantum dots (N-GQDs) with greenish-yellow emission and quantum yield of 13.2% have been synthesized via a one-pot hydrothermal method. The obtained N-GQDs displayed excellent optical properties, high photostability and resistance to strong ion strength. Based on the higher affinity of pyrophosphate (PPi) than carboxyl and amido groups on the surface of the N-GQDs to Eu(3+), a Eu(3+)-modulated N-GQD off-on fluorescent probe for PPi detection was constructed with a detection limit of 0.074 μM. The detection process was simple in design, easy to operate, and showed a highly selective response to PPi in the presence of co-existing anions. This work widens the applications of N-GQDs with versatile functionality and reactivity in clinical diagnostics and as biosensors.