Synthesis and analgetic activity of 1,2,3,4,5,6-hexahydro-1,6-methano-3-benzozocines.

PubMed

Mazzocchi, P H; Harrison, A M

1978-02-01

1,2,3,4,5,6-Hexahydro-1,6-methano-3-benzazocine (1) has been synthesized via a four-step sequence from benzo-norbornadiene. This compound and its N-methyl derivative are more active than codeine in the mouse hot-plate antinociceptive assay and will not suppor morphine dependence in Rhesus monkeys.

New Sulfide Compounds MeXMn1-XS (Me=3d Metal) with the Colossal Magnetoresistance Effect

DTIC Science & Technology

2006-05-19

is to synthesize the new MeXMn1-XS (Me=3d-metal) sulfide compounds and to study the electrical, magnetic and magnetoresistive properties . Recently...oxide compounds of manganese (LaMnO3-type) with perovskite structure have been intensively investigated. This interest is caused by the observation of... properties of the materials with different structure. It is known that alpha - MnS manganese monosulfide, similar to LaMnO3, has the specific

Superconductivity in LaCu 6 and possible applications

NASA Astrophysics Data System (ADS)

Herrmannsdörfer, Thomas; Pobell, Frank; Sebek, Josef; Svoboda, Pavel

2003-05-01

We have measured the ac susceptibility and resistivity of highly pure samples of the intermetallic compound LaCu6 down to ultralow temperatures. We have prepared the samples by arc melting of stoichiometric amounts of 99.99% La and 99.9999% Cu in a water-cooled copper crucible under Ar protective atmosphere and analysed them by X-ray diffraction and SQUID magnetometry. At T⩽Tc=0.16 K we observe a superconducting transition. Due to the manifold physical properties of isostructural ReCu6 compounds (e.g. RE = Ce: heavy fermion system, RE=Pr: hyperfine enhanced nuclear spin system, RE = Nd: electronic antiferromagnet), numerous studies of interplay phenomena may become possible in the quasibinary compounds RE1-xLaxCu6, respectively.

Synthesis and X-ray structural investigation of (5R*,6S*)-1-benzoyl-5-methylthio-6-methoxy-1-azapenam

NASA Astrophysics Data System (ADS)

Krajewski, J. W.; Gluziński, P.; Grochowski, E.; Pupek, K.; Mishnyov, A.; Kemme, A.

1992-08-01

The compound (5R*,6S*)-1-benzoyl-5-methylthio-6-methoxy-1-azapenam ( 3) has been synthesized and its structure investigated by X-ray diffraction. The compound crystallizes in a monoclinic system, space group Cc, Z = 4, a = 12.01(1), b = 16.51(1), c = 8.048(6) Å, β = 115.87(6)°. The structure was solved by direct methods and refined by a full-matrix, least-squares procedure to give R = 0.070, Rw = 0.046, w = 1.34/(σ 2F). The expected cis configuration around the β-lactam ring was fully confirmed.

The Crystal Structure and Magnetic Behavior of Quinary Osmate and Ruthenate Double Perovskites La ABB'O 6 ( A = Ca, Sr; B = Co, Ni; B' = Ru, Os)

DOE PAGES

Morrow, Ryan; McGuire, Michael A.; Yan, Jiaqiang; ...

2018-02-23

In this work, six LaABB'O 6 (A = Ca, Sr; B = Co, Ni; B' = Ru, Os) double perovskites were synthesized, several for the first time, and their crystal structures and magnetic behavior were characterized with neutron powder diffraction and direct-current and alternating-current magnetometry. All six compounds crystallize with P2 1/n space group symmetry, resulting from a –a –c + octahedral tilting and complete rock salt ordering of transition-metal ions. Despite the electronic configurations of the transition-metal ions, either d 8–d 3 or d 7–d 3, not one of the six compounds shows ferromagnetism as predicted by the Goodenough–Kanamorimore » rules. LaSrNiOsO 6, LaSrNiRuO 6, and LaCaNiRuO 6 display long-range antiferromagnetic order, while LaCaNiOsO 6, LaCaCoOsO 6, and LaSrCoOsO 6 exhibit spin-glass behavior. These compounds are compared to the previously studied LaCaCoRuO 6 and LaSrCoRuO 6, both of which order antiferromagnetically. Lastly, the observed variations in magnetic properties can be attributed largely to the response of competing superexchange pathways due to changes in B–O–B' bond angles, differences in the radial extent of the 4d (B' = Ru) and 5d (B' = Os) orbitals, and filling of the t 2g orbitals of the 3d ion.« less

The Crystal Structure and Magnetic Behavior of Quinary Osmate and Ruthenate Double Perovskites La ABB'O 6 ( A = Ca, Sr; B = Co, Ni; B' = Ru, Os)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Morrow, Ryan; McGuire, Michael A.; Yan, Jiaqiang

In this work, six LaABB'O 6 (A = Ca, Sr; B = Co, Ni; B' = Ru, Os) double perovskites were synthesized, several for the first time, and their crystal structures and magnetic behavior were characterized with neutron powder diffraction and direct-current and alternating-current magnetometry. All six compounds crystallize with P2 1/n space group symmetry, resulting from a –a –c + octahedral tilting and complete rock salt ordering of transition-metal ions. Despite the electronic configurations of the transition-metal ions, either d 8–d 3 or d 7–d 3, not one of the six compounds shows ferromagnetism as predicted by the Goodenough–Kanamorimore » rules. LaSrNiOsO 6, LaSrNiRuO 6, and LaCaNiRuO 6 display long-range antiferromagnetic order, while LaCaNiOsO 6, LaCaCoOsO 6, and LaSrCoOsO 6 exhibit spin-glass behavior. These compounds are compared to the previously studied LaCaCoRuO 6 and LaSrCoRuO 6, both of which order antiferromagnetically. Lastly, the observed variations in magnetic properties can be attributed largely to the response of competing superexchange pathways due to changes in B–O–B' bond angles, differences in the radial extent of the 4d (B' = Ru) and 5d (B' = Os) orbitals, and filling of the t 2g orbitals of the 3d ion.« less

High potential thermoelectric figure of merit in ternary La 3Cu 3X 4 (X = P, As, Sb and Bi) compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pandey, Tribhuwan; Parker, David S.

Here, we investigate the thermoelectric properties of the relatively unexplored rare-earth ternary compounds La 3Cu 3X 4 (X= Bi, Sb, As, and P) using first principles electronic structure and Boltzmann transport calculations. These compounds, of which the La 3Cu 3Sb 4 and La 3Cu 3Bi 4 compounds have previously been synthesized, are all predicted to semiconductors and present a wide range of band gaps varying from 0.23 eV (for the Bi compound) to 0.87 eV (for the P compound). We further find a mixture of light and heavy bands, which results in a high thermoelectric power factor. In addition wemore » find that at high temperatures of 1000 K these compounds exhibit lattice thermal conductivity less than 1 W/m-K. The combination of low thermal conductivity and good transport properties results in a predicted ZT as high as ~1.5 for both La 3Cu 3P 4 and La 3Cu 3As 4, under high p-type doping. This predicted high performance makes these compounds promising candidates for high performance thermoelectric performance and thus merits further experimental investigation.« less

High potential thermoelectric figure of merit in ternary La 3Cu 3X 4 (X = P, As, Sb and Bi) compounds

DOE PAGES

Pandey, Tribhuwan; Parker, David S.

2017-10-27

Here, we investigate the thermoelectric properties of the relatively unexplored rare-earth ternary compounds La 3Cu 3X 4 (X= Bi, Sb, As, and P) using first principles electronic structure and Boltzmann transport calculations. These compounds, of which the La 3Cu 3Sb 4 and La 3Cu 3Bi 4 compounds have previously been synthesized, are all predicted to semiconductors and present a wide range of band gaps varying from 0.23 eV (for the Bi compound) to 0.87 eV (for the P compound). We further find a mixture of light and heavy bands, which results in a high thermoelectric power factor. In addition wemore » find that at high temperatures of 1000 K these compounds exhibit lattice thermal conductivity less than 1 W/m-K. The combination of low thermal conductivity and good transport properties results in a predicted ZT as high as ~1.5 for both La 3Cu 3P 4 and La 3Cu 3As 4, under high p-type doping. This predicted high performance makes these compounds promising candidates for high performance thermoelectric performance and thus merits further experimental investigation.« less

Successive magnetic transitions of the pseudo-ternary compounds Ho1-xRxRh2Si2 (R=Y, La)

NASA Astrophysics Data System (ADS)

Shigeoka, Toru; Uchima, Kiyoharu; Uwatoko, Yoshiya

2018-05-01

Magnetic measurements on the pseudo-ternary compounds Ho1-xRxRh2Si2 (R = Y or La = Y or La) were performed in order to get information on the origin of "the successive component-separated magnetic transitions" which appear in HoRh2Si2. The lattice parameters a and c remain almost constant during changes to Y composition x, while they increase with increasing La composition x. The c/a ratios are also constant in the Y-system, and they increase with increasing x in the La-system especially for above around x = 0.4. The transition temperatures, TN1 = 29.1 K, Tt = 27.3 K and TN2 =12.1 K at x = 0, decrease with increasing x. The rates of decrease for TN1 and TN2 in the Y-system accord with those in the La system below x = 0.4. The critical compositions for TN1 and TN2 are determined to be xN1 = 0.88 and xN2 = 0.59 in the La-system, respectively, and xN1 = 0.98 and xN2 = 0.75 in the Y-system. In both the systems, "the successive component-separated magnetic transitions" appear for the wide x regions. The magnetic ordered state persists in very dilute Ho-compounds in spite of much weak magnetic interactions. The effective magnetic moments are almost constant for the ordered compounds; μeff = 10.6 ± 0.30 μB/Ho. These behaviors are strange, indicating a strong correlation exists in these systems.

Evaluation of the magnetocaloric response of nano-sized La0.7Ca0.3Mn1-xNixO3 manganites synthesized by auto-combustion method

NASA Astrophysics Data System (ADS)

Gómez, Adrián; Chavarriaga, Edgar; Supelano, Iván; Parra, Carlos Arturo; Morán, Oswaldo

2018-05-01

A systematic study of the dependence of the magnetization on the magnetic field around the ferromagnetic-paramagnetic phase transition temperature is carried out on La0.7Ca0.3Mn1-xNixO3 (x=0, 0.02, 0.07, and 1) samples synthesized by auto-combustion method. The successful substitution of Mn3+ ions by Ni2+ ions in the La0.7Ca0.3MnO3 lattice is corroborated by X-ray diffraction technique. Banerjees criteria, Arrott plots, and the scaling hypothesis are used to analyze the experimental data. It is verified that the Ni-doping increases the operating temperature range for magnetocaloric effect through tuning of the magnetic transition temperature. Probably, the replacement of Mn3+ by Ni2+ ions in the La0.7Ca0.3MnO3 lattice weakens the Mn3+-O-Mn4+ double exchange interaction, which leads to a decrease in the transition temperature and magnetic moment in the samples. The Arrott plots suggest that the phase transition from ferromagnetic to paramagnetic in the nano-sized manganite is of second order. The analysis of the magnetization results show that the maximum magnetic entropy changes observed for x=0, 0.02, 0.07, and 0.1 compositions are 0.85, 0.77, 0.63, and 0.59 J/kg K, under a magnetic field of 1.5 T. These values indicate that the magnetic entropy change achieved for La0.7Ca0.3Mn1-xNixO3 manganites synthesized by auto-combustion method is higher than those reported for other manganites with comparable Ni-doping levels but synthesized by standard solid state reaction. It is also observed that the addition of Ni2+ increases the value of the relative cooling power as compared to that of the parent compound. The highest value of this parameter (˜60 J/kg) is found for a Ni-doping level of 2 % around 230 K in a field of 1.5 T.

SYNTHESIZING ORGANIC COMPOUNDS USING LIGHT-ACTIVATED TIO2

EPA Science Inventory

High-value organic compounds have been synthesized successfully from linear and cyclic hydrocarbons, by photocatalytic oxidation using a semiconductor material, titanium dioxide (TiO2). Various hydrocarbons were partially oxgenated in both liquid and gaseous phase reactors usi...

Search for Compounds with Hypoglycemic Activity in the Series of 1-[2-(1H-Tetrazol-5-yl)-R1-phenyl]-3-R2-phenyl(ethyl)ureas and R1-Tetrazolo[1,5-c]quinazolin-5(6H)-ones

PubMed Central

Antypenko, Oleksii M.; Kovalenko, Sergiy I.; Zhernova, Galina O.

2016-01-01

Methods of 1-[2-(1H-tetrazol-5-yl)-R1-phenyl]-3-R2-phenyl(ethyl)ureas and R1-tetrazolo[1,5-c]quinazolin-5(6H)-ones synthesis were designed. IR, LC-MS, 1H NMR, and elemental analysis data evaluated the structure and purity of the obtained compounds. Different products, depending on the reaction conditions, were distinguished and discussed. The preliminary hypoglycemic activity of 36 synthesized compounds was revealed. Docking studies to 11β-hydroxysteroid dehydrogenase 1, γ-peroxisome proliferator-activated receptor, and dipeptidyl peptidase-4 were conducted. Eight of these substances were further tested on glucocorticoid-induced insulin resistance models, namely glucose tolerance, oral rapid insulin, and adrenalin tests. One of the most active compounds turned out to be tetrazolo[1,5-c]quinazolin-5(6H)-one 3.1, exceeding the reference drugs Metformin (50 and 200 mg/kg) and Gliclazide (50 mg/kg). PMID:27222601

Cytotoxic activity of proflavine diureas: synthesis, antitumor, evaluation and DNA binding properties of 1',1''-(acridin-3,6-diyl)-3',3''-dialkyldiureas.

PubMed

Kozurková, Mária; Sabolová, Danica; Janovec, Ladislav; Mikes, Jaromír; Koval', Ján; Ungvarský, Ján; Stefanisinová, Miroslava; Fedorocko, Peter; Kristian, Pavol; Imrich, Ján

2008-04-01

The synthesis of novel 1',1''-(acridin-3,6-diyl)-3',3''-dialkyldiureas was reported. Their biological activity to inhibit cell proliferation was assessed by a MTT assay on two cell lines, HeLa and HCT-116, at micromolar concentration. 1',1''-(Acridin-3,6-diyl)-3',3''-dihexyldiurea hydrochloride was active on a HCT-116 cell line with an IC(50) value of 3.1 microM. The interaction of these compounds with calf thymus DNA was investigated by a variety of spectroscopic techniques including UV-vis, fluorescence and CD spectroscopy. From spectrofluorimetric titrations, binding constants for the DNA-drug complexes were determined (K=0.9-4.2x10(5) M(-1)). Antiproliferative activity of synthesized derivatives might be related to their intercalation into DNA.

6. Photocopy of architectural blueprint (on file at the La ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

6. Photocopy of architectural blueprint (on file at the La Grande District Office, La Grande, Oregon) USDA Forest Service, 1938 GUARD RESIDENCE (SHEET 1 OF 4) - Union Ranger District Compound, Guard Residence, Fronting State Highway 203, at West edge of Union, Union, Union County, OR

Penicillins and other acylamino compounds synthesized by the cell-bound penicillin acylase of Escherichia coli

PubMed Central

Cole, M.

1969-01-01

1. The penicillin acylase of Eschericha coli N.C.I.B. 8743 is a reversible enzyme. Reaction rates for the two directions have been determined. 2. Measurements of the rates of enzymic synthesis of penicillins from 6-aminopenicillanic acid and various carboxylic acids revealed that p-hydroxyphenylacetic acid was the best substrate, followed by phenylacetic, 2-thienylacetic, substituted phenylacetic, 3-hexenoic and n-hexanoic acids. 3. The rate of synthesis of penicillin improved when amides or N-acylglycines were used; α-aminobenzylpenicillin and phenoxymethylpenicillin were only synthesized when using these more energy-rich compounds. 4. Phenyl-acetylglycine was the best substrate for the synthesis of benzylpenicillin compared with other derivatives of phenylacetic acid. 5. The enzyme was specific for acyl-l-amino acids, benzylpenicillin being synthesized from phenylacetyl-l-α-aminophenylacetic acid but not from phenylacetyl-d-α-aminophenylacetic acid. 6. α-Phenoxyethylpenicillin was synthesized from 6-aminopenicillanic acid and α-phenoxypropionylthioglycollic acid non-enzymically, but the rate was faster in the presence of the enzyme. 7. The E. coli acylase catalysed the acylation of hydroxylamine by acids or amides to give hydroxamic acids, the phenylacetyl group being the most suitable acyl group. The enzyme also catalysed other acyl-group transfers. PMID:4982418

Pentavalent and tetravalent uranium selenides, Tl3Cu4USe6 and Tl2Ag2USe4: syntheses, characterization, and structural comparison to other layered actinide chalcogenide compounds.

PubMed

Bugaris, Daniel E; Choi, Eun Sang; Copping, Roy; Glans, Per-Anders; Minasian, Stefan G; Tyliszczak, Tolek; Kozimor, Stosh A; Shuh, David K; Ibers, James A

2011-07-18

The compounds Tl(3)Cu(4)USe(6) and Tl(2)Ag(2)USe(4) were synthesized by the reaction of the elements in excess TlCl at 1123 K. Both compounds crystallize in new structure types, in space groups P2(1)/c and C2/m, respectively, of the monoclinic system. Each compound contains layers of USe(6) octahedra and MSe(4) (M = Cu, Ag) tetrahedra, separated by Tl(+) cations. The packing of the octahedra and the tetrahedra within the layers is compared to the packing arrangements found in other layered actinide chalcogenides. Tl(3)Cu(4)USe(6) displays peaks in its magnetic susceptibility at 5 and 70 K. It exhibits modified Curie-Weiss paramagnetic behavior with an effective magnetic moment of 1.58(1) μ(B) in the temperature range 72-300 K, whereas Tl(2)Ag(2)USe(4) exhibits modified Curie-Weiss paramagnetic behavior with μ(eff) = 3.4(1) μ(B) in the temperature range 100-300 K. X-ray absorption near-edge structure (XANES) results from scanning transmission X-ray spectromicroscopy confirm that Tl(3)Cu(4)USe(6) has Se bonding characteristic of discrete Se(2-) units, Cu bonding generally representative of Cu(+), and U bonding consistent with a U(4+) or U(5+) species. On the basis of these measurements, as well as bonding arguments, the formal oxidation states for U may be assigned as +5 in Tl(3)Cu(4)USe(6) and +4 in Tl(2)Ag(2)USe(4).

Synthesis of Some Novel Fused Pyrimido[4″,5″:5',6']-[1,2,4]triazino[3',4':3,4] [1,2,4]triazino[5,6-b]indoles with Expected Anticancer Activity.

PubMed

Ali, Rania S; Saad, Hosam A

2018-03-19

Our current goal is the synthesis of polyheterocyclic compounds starting from 3-amino-[1,2,4]triazino[5,6- b ]indole 1 and studying their anticancer activity to determine whether increasing of the size of the molecules increases the anticancer activity or not. 1-Amino[1,2,4]triazino[3',4':3,4]-[1,2,4]triazino[5,6- b ]indole-2-carbonitrile ( 4 ) was prepared by the diazotization of 3-amino[1,2,4]-triazino[5,6- b ]indole 1 followed by coupling with malononitrile in basic medium then cyclization under reflux to get 4 . Also, new fused pyrimido[4″,5″:5',6'][1,2,4]triazino-[3',4':3,4][1,2,4]triazino[5,6- b ]indole derivative 6 was prepared and used to obtain polycyclic heterocyclic systems. Confirmation of the synthesized compounds' structures was carried out using elemental analyses and spectral data (IR, ¹H-NMR and 13 C-NMR and mass spectra). The anticancer activity of some of the synthesized compounds was tested against HepG2, HCT-116 and MCF-7 cell lines. The anticancer screening results showed that some derivatives display good activity which was more potent than that of the reference drug used. Molecular docking was used to predict the binding between some of the synthesized compounds and the prostate cancer 2q7k hormone and breast ‎cancer 3hb5 receptors.

Process for synthesizing compounds from elemental powders and product

DOEpatents

Rabin, Barry H.; Wright, Richard N.

1993-01-01

A process for synthesizing intermetallic compounds from elemental powders. The elemental powders are initially combined in a ratio which approximates the stoichiometric composition of the intermetallic compound. The mixed powders are then formed into a compact which is heat treated at a controlled rate of heating such that an exothermic reaction between the elements is initiated. The heat treatment may be performed under controlled conditions ranging from a vacuum (pressureless sintering) to compression (hot pressing) to produce a desired densification of the intermetallic compound. In a preferred form of the invention, elemental powders of Fe and Al are combined to form aluminide compounds of Fe.sub.3 Al and FeAl.

Nanocrystalline Ce1- x La x O2- δ Solid Solutions Synthesized by Hydrolyzing and Oxidizing

NASA Astrophysics Data System (ADS)

Hou, Xueling; Xue, Yun; Han, Ning; Lu, Qianqian; Wang, Xiaochen; Phan, Manh-Huong; Zhong, Yunbo

2016-05-01

We undertook a novel batch production approach for the synthesis of CeO2 nanopowders doped with rare earth elements. Solid solution nanopowders of Ce1- x La x O2- δ ( x = 0.15) were successfully synthesized in a large-scale and low-cost production by hydrolyzing and oxidizing Ce-La-C alloys at room temperature and subsequent calcining of their powders at different temperatures (873-1073 K) for 1 h. The Ce-La-C alloys were prepared in a vacuum induction melting furnace. The final products were characterized by x-ray diffraction, transmission electron microscopy, Brunner-Emmet-Teller (BET) surface area analyzer, and Raman spectroscopy. The calculated lattice parameters of the cubic fluorite-type phase of CeO2 tended to increase when La3+ was incorporated into CeO2. The F 2g band shift and the absence of a peak corresponding to La2O3 in the Raman spectra consistently confirmed the incorporation of the La3+ ion into CeO2, and the formation of Ce1- x La x O2- δ solid solutions as manifested by increased oxygen vacancy defects. High-quality Ce1- x La x O2- δ nanopowders of ~10-15 nm diameter with a high BET surface area of ~77 m2 g-1 were obtained. The average crystallite size of Ce1- x La x O2- δ was found to be smaller than that of CeO2 for the same calcination temperature of 1073 K, demonstrating that the introduction of La3+ into CeO2 can stabilize the host lattice and refine the grain size at high temperatures.

Synthesis, characterization and spectroscopic behavior of novel 2-oxo-1,4-disubstituted-1,2,5,6-tetrahydrobenzo[h]quinoline-3-carbonitrile dyes.

PubMed

Khan, Salman A; Asiri, Abdullah M; Al-Thaqafy, Saad H; Faidallah, Hassan M; El-Daly, Samy A

2014-12-10

Two synthetic pathways were adopted to synthesize the target 2-oxo-1,4-disubstituted-1,2,5,6-tetrahydro-benzo[h]quinoline-3-carbonitriles. Structure of the synthesized compounds has been characterized based on FT-IR, (1)H NMR, (13)C NMR and elemental analyses. UV-Vis and fluorescence spectroscopy measurements provided that all compounds are good absorbent and fluorescent. Fluorescence polarity study demonstrated that these compounds were sensitive to the polarity of the microenvironment provided by different solvents. In addition, spectroscopic and physicochemical parameters, including singlet absorption, extinction coefficient, Stokes shift, oscillator strength and dipole moment were investigated in order to explore the analytical potential of synthesized compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

Syntheses of 4,6-dihydroxypyrimidine diones, their urease inhibition, in vitro, in silico, and kinetic studies.

PubMed

Muhammad, Munira Taj; Khan, Khalid Mohammed; Arshia; Khan, Ajmal; Arshad, Fiza; Fatima, Bibi; Choudhary, M Iqbal; Syed, Naima; Moin, Syed Tarique

2017-12-01

A library of 4,6-dihydroxypyrimidine diones (1-35) were synthesized and evaluated for their urease inhibitory activity. Structure-activity relationships, and mechanism of inhibition were also studied. All compounds were found to be active with IC 50 values between 22.6±1.14-117.4±0.73µM, in comparison to standard, thiourea (IC 50 =21.2±1.3µM). Kinetics studies on the most active compounds 2-7, 16, 17, 28, and 33 were performed to investigate their modes of inhibition, and dissociation constants K i . Compounds 2, 3, 7, 16, 28, and 33 were found to be mixed-type of inhibitors with K i values in the range of 7.91±0.024-13.03±0.013µM, whereas, compounds 4-6, and 17 were found to be non-competitive inhibitors with K i values in the range of 9.28±0.019-13.05±0.023µM. In silico study was also performed, and a good correlation was observed between experimental and docking studies. This study is continuation of our previously reported urease inhibitory activity of pyrimidine diones, representing potential leads for further research as possible treatment of diseases caused by ureolytic bacteria. Copyright © 2017. Published by Elsevier Inc.

Synthesis and cytotoxic evaluation of some new 4(3H)-quinazolinones on HeLa cell line

PubMed Central

Khodarahmi, G.A.; Shamshiri, M.; Hassanzadeh, F.

2012-01-01

Quinazolinone backbone is present in a large number of bioactive substances. Since remarkable cytotoxic activity is associated with some 4(3H)-quinazolinones, in this study some 4(3H)-quinazolinone were synthesized and screened against HeLa cells. The synthesis was performed via reaction of anthranilic acid with dicarboxylic anhydrides to produce carboxylic acids derivatives. The products were heated in acetic anhydride to produce benzoxazinones. Finally, 4(3H)-quinazolinones were synthesized by reaction between benzoxazinones and primary amines. The assessment of the structure of the synthesized compounds was based on spectral data (FT-IR, Mass and 1HNMR). Subsequently, cytotoxic activity of compounds 3, 6, 9 and 13 (individually and in combination with doxorubicin) was evaluated on HeLa cell line using MTT assay. The results indicated that the tested compounds did not show significant cytotoxicity alone and in combination with doxorubicin (1 and 20 μM). PMID:23181089

Metal ion displacements in noncentrosymmetric chalcogenides La{sub 3}Ga{sub 1.67}S{sub 7}, La{sub 3}Ag{sub 0.6}GaCh{sub 7} (Ch=S, Se), and La{sub 3}MGaSe{sub 7} (M=Zn, Cd)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Iyer, Abishek K.; Yin, Wenlong; Institute of Chemical Materials, China Academy of Engineering Physics, Mianyang 621900

The quaternary Ga-containing chalcogenides La{sub 3}Ag{sub 0.6}GaS{sub 7}, La{sub 3}Ag{sub 0.6}GaSe{sub 7}, La{sub 3}ZnGaSe{sub 7}, and La{sub 3}CdGaSe{sub 7}, as well as the related ternary chalcogenide La{sub 3}Ga{sub 1.67}S{sub 7}, were prepared by reactions of the elements at 950 °C. They adopt noncentrosymmetric hexagonal structures (space group P6{sub 3}, Z=2) with cell parameters (a=10.2 Å, c=6.1 Å for the sulfides; a=10.6 Å, c=6.4 Å for the selenides) that are largely controlled by the geometrical requirements of one-dimensional stacks of Ga-centered tetrahedra separated by the La atoms. Among these compounds, which share the common formulation La{sub 3}M{sub 1–x}GaCh{sub 7} (M=Ga, Ag,more » Zn, Cd; Ch=S, Se), the M atoms occupy sites within a stacking of trigonal antiprisms formed by Ch atoms. The location of the M site varies between extremes with trigonal antiprismatic (CN6) and trigonal planar (CN3) geometry. Partial occupation of these sites and intermediate ones accounts for the considerable versatility of these structures and the occurrence of large metal displacement parameters. The site occupations can be understood in a simple way as being driven by the need to satisfy appropriate bond valence sums for both the M and Ch atoms. Band structure calculations rationalize the substoichiometry observed in the Ag-containing compounds (La{sub 3}Ag{sub 0.6}GaS{sub 7}, La{sub 3}Ag{sub 0.6}GaSe{sub 7}) as a response to overbonding. X-ray photoelectron spectroscopy supports the presence of monovalent Ag atoms in these compounds, which are not charge-balanced. - Graphical abstract: Partial occupation of metal atoms in multiple sites accounts for versatility in Ga-containing chalcogenides La{sub 3}M{sub 1–x}GaCh{sub 7} with noncentrosymmetric hexagonal structures. - Highlights: • La{sub 3}M{sub 1–x}GaCh{sub 7} (M =Ga, Ag, Zn, Cd; Ch =S, Se) adopt related hexagonal structures. • Large displacements of M atoms originate from partial occupation of

Process for synthesizing compounds from elemental powders and product

DOEpatents

Rabin, B.H.; Wright, R.N.

1993-12-14

A process for synthesizing intermetallic compounds from elemental powders is described. The elemental powders are initially combined in a ratio which approximates the stoichiometric composition of the intermetallic compound. The mixed powders are then formed into a compact which is heat treated at a controlled rate of heating such that an exothermic reaction between the elements is initiated. The heat treatment may be performed under controlled conditions ranging from a vacuum (pressureless sintering) to compression (hot pressing) to produce a desired densification of the intermetallic compound. In a preferred form of the invention, elemental powders of Fe and Al are combined to form aluminide compounds of Fe[sub 3] Al and FeAl. 25 figures.

New effective chemically synthesized anti-smallpox compound NIOCH-14.

PubMed

Mazurkov, Oleg Yu; Kabanov, Alexey S; Shishkina, Larisa N; Sergeev, Alexander A; Skarnovich, Maksim O; Bormotov, Nikolay I; Skarnovich, Maria A; Ovchinnikova, Alena S; Titova, Ksenya A; Galahova, Darya O; Bulychev, Leonid E; Sergeev, Artemiy A; Taranov, Oleg S; Selivanov, Boris A; Tikhonov, Alexey Ya; Zavjalov, Evgenii L; Agafonov, Alexander P; Sergeev, Alexander N

2016-05-01

Antiviral activity of the new chemically synthesized compound NIOCH-14 (a derivative of tricyclodicarboxylic acid) in comparison with ST-246 (the condensed derivative of pyrroledione) was observed in experiments in vitro and in vivo using orthopoxviruses including highly pathogenic ones. After oral administration of NIOCH-14 to outbred ICR mice infected intranasally with 100 % lethal dose of ectromelia virus, it was shown that 50 % effective doses of NIOCH-14 and ST-246 did not significantly differ. The 'therapeutic window' varied from 1 day before infection to 6 days post-infection (p.i.) to achieve 100-60 % survival rate. The administration of NIOCH-14 and ST-246 to mice resulted in a significant reduction of ectromelia virus titres in organs examined as compared with the control and also reduced pathological changes in the lungs 6 days p.i. Oral administration of NIOCH-14 and ST-246 to ICR mice and marmots challenged with monkeypox virus as compared with the control resulted in a significant reduction of virus production in the lungs and the proportion of infected mice 7 days p.i. as well as the absence of disease in marmots. Significantly lower proportions of infected mice and virus production levels in the lungs as compared with the control were demonstrated in experiments after oral administration of NIOCH-14 and ST-246 to ICR mice and immunodeficient SCID mice challenged with variola virus 3 and 4 days p.i., respectively. The results obtained suggest good prospects for further study of the chemical compound NIOCH-14 to create a new smallpox drug on its basis.

Pharmacological properties of pempidine (1:2:2:6:6-pentamethylpiperidine), a new ganglion-blocking compound

PubMed Central

Corne, S. J.; Edge, N. D.

1958-01-01

Pempidine (1:2:2:6:6-pentamethylpiperidine) is a long-acting ganglion-blocking compound which is effective by mouth. By intravenous injection it has a similar potency to hexamethonium on the preganglionically stimulated nictitating membrane of the cat. The compound blocks the effects of intravenous nicotine and of peripheral vagal stimulation on the blood pressure; it also causes dilatation of the pupil after removal of the sympathetic innervation. On the guinea-pig ileum, the predominant effect of the compound is to inhibit nicotine contractions. Pempidine is well absorbed from the gastro-intestinal tract as judged by (a) the low ratio (6.9) of oral to intravenous toxicities, (b) the rapid development of mydriasis in mice after oral administration of small doses, and (c) the rapid onset of hypotension when the compound is injected directly into the duodenum of anaesthetized cats. Other actions include neuromuscular paralysis of curare-like type when large doses of the compound are injected intravenously and central effects such as tremors which occur with near toxic doses. In cats with a low blood pressure, large intravenous doses have a slight pressor action. PMID:13584741

Effect of strontium substitution on the structural and magnetic properties of La1.8Sr0.2MMnO6 (M = Ni, Co)-layered manganites

NASA Astrophysics Data System (ADS)

Karimunnesa, Syeda; Ahmmad, Bashir; Basith, M. A.

2017-07-01

Sr-substituted perovskites, La1.8Sr0.2MMnO6 (M = Ni, Co), were synthesized using the solid-state reaction technique to present a systematic study on their morphological, structural and magnetic properties. The average grain size of the as-prepared La1.8Sr0.2NiMnO6 samples are in the range of 0.2-0.7 µm and those for La1.8Sr0.2CoMnO6 manganites are 0.1-2.8 μm, which is significantly less than that of unsubstituted La2NiMnO6 (LNMO) and La2CoMnO6 (LCMO) manganites. The XPS analysis enlightened about phase purity, binding energy and oxygen vacancy of La1.8Sr0.2MMnO6 manganites. The Sr-substituted LNMO has revealed a sharp ferromagnetic to paramagnetic phase transition at 160 ± 2 K, which is about 120 K less than that of parent LNMO. The Sr-substituted LCMO exhibited such a transition at 220 ± 2 K, which is 8 K less than that of parent LCMO. The temperature-dependent magnetization measurements suggest that the effect of Sr on the transition temperature in LNMO is more significant than that of LCMO.

Syntheses, structures and properties of two new coordination polymers based on D-camphoric acid and 2-phenyl-4,6-diamino-1,3,5-triazine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lun, Huijie; Yang, Jinghe; Jin, Linyu

2015-05-15

By hydrothermal method, two new coordination polymers [Co(ca)(phdat)]{sub n} (1), [Ni(ca)(phdat).0.125H{sub 2}O]{sub n} (2) (H{sub 2}ca=D-camphoric acid, phdat=2-phenyl-4,6-diamino-1,3,5-triazine) have been achieved and structurally characterized by IR, elemental analyses, X-ray single-crystal diffraction and TGA. The X-ray single-crystal diffraction reveals that compounds 1 and 2 are isostructural, both of which exhibit two-dimensional layered network built up from paddle-wheel Co{sub 2}(CO{sub 2}){sub 4}/Ni{sub 2}(CO{sub 2}){sub 4} SBUs by ca{sup 2−} ligand. In the existence of π…π stacking interactions between triazine rings and phenyl rings, the 3D networks are constructed with the hanging phdat filled between the neighboring layers. Furthermore, compounds 1–2 exhibit antiferromagneticmore » behavior and compound 2 displays a good activity for methanol oxidation. - Graphical abstract: Two new coordination compounds 1–2 have been synthesized and characterized by single-crystal X-ray diffractions, IR spectra, elemental analyses, thermogravimetric analyses, magnetic and electrochemical measurement. - Highlights: • This paper reports two new coordination polymers based on D-camphoric acid. • Both the compounds feather two-dimensional layered networks built up from paddle-wheel SBUs. • The magnetism and electrochemical property are investigated.« less

Novel Tandem Biotransformation Process for the Biosynthesis of a Novel Compound, 4-(2,3,5,6-Tetramethylpyrazine-1)-4′-Demethylepipodophyllotoxin▿

PubMed Central

Tang, Ya-Jie; Zhao, Wei; Li, Hong-Mei

2011-01-01

According to the structure of podophyllotoxin and its structure-function relationship, a novel tandem biotransformation process was developed for the directional modification of the podophyllotoxin structure to directionally synthesize a novel compound, 4-(2,3,5,6-tetramethylpyrazine-1)-4′-demethylepipodophyllotoxin (4-TMP-DMEP). In this novel tandem biotransformation process, the starting substrate of podophyllotoxin was biotransformed into 4′-demethylepipodophyllotoxin (product 1) with the demethylation of the methoxyl group at the 4′ position by Gibberella fujikuroi SH-f13, which was screened out from Shennongjia prime forest humus soil (Hubei, China). 4′-Demethylepipodophyllotoxin (product 1) was then biotransformed into 4′-demethylpodophyllotoxone (product 2) with the oxidation of the hydroxyl group at the 4 position by Alternaria alternata S-f6, which was screened out from the gathered Dysosma versipellis plants in the Wuhan Botanical Garden, Chinese Academy of Sciences. Finally, 4′-demethylpodophyllotoxone (product 2) and ligustrazine were linked with a transamination reaction to synthesize the target product 4-TMP-DMEP (product 3) by Alternaria alternata S-f6. Compared with podophyllotoxin (i.e., a 50% effective concentration [EC50] of 529 μM), the EC50 of 4-TMP-DMEP against the tumor cell line BGC-823 (i.e., 0.11 μM) was significantly reduced by 5,199 times. Simultaneously, the EC50 of 4-TMP-DMEP against the normal human proximal tubular epithelial cell line HK-2 (i.e., 0.40 μM) was 66 times higher than that of podophyllotoxin (i.e., 0.006 μM). Furthermore, compared with podophyllotoxin (i.e., log P = 0.34), the water solubility of 4-TMP-DMEP (i.e., log P = 0.66) was significantly enhanced by 94%. For the first time, the novel compound 4-TMP-DMEP with superior antitumor activity was directionally synthesized from podophyllotoxin by the novel tandem biotransformation process developed in this work. PMID:21398491

Experimental and theoretical analysis of a rare nitrato bridged 3d-4f complex containing LaZn2 core synthesized from a Zn(II) metalloligand

NASA Astrophysics Data System (ADS)

Sreejith, S. S.; Mohan, Nithya; Kurup, M. R. Prathapachandra

2018-02-01

A trinulcear Zn2La Schiff base complex was synthesized using slow-solvent evaporation technique from a Zn(II) mononuclear metalloligand by 2:1 addition with La(NO3)3 salt. Single crystal XRD analysis revealed a rare nitrato bridged trinuclear entity which is seldom seen in these class of ligand systems. Qualitative and quantitative analysis of intermolecular interactions/short contacts were done using Hirshfeld surface and 2D finger print analysis. The thermally stable, blue luminescent compound exhibits internal heavy atom effect thereby quenching the emission intensity of the ligand. DFT calculations were performed on the compound to analyze frontier orbitals and also ESP plots were used to monitor nucleophilic/electrophilic regions on the compound and its implications on hydrogen bonding. A comparison of the bond orders and atomic charges on the trinuclear compound and the Zn(II) metalloligand precursor was performed to substantiate the formation of the trinuclear product through ligand exchange.

Novel amide and sulphonamide derivatives of 6-(piperazin-1-yl)phenanthridine as potent Mycobacterium tuberculosis H37Rv inhibitors.

PubMed

Naidu, Kalaga Mahalakshmi; Nagesh, Hunsur Nagendra; Singh, Manjeet; Sriram, Dharmarajan; Yogeeswari, Perumal; Gowri Chandra Sekhar, Kondapalli Venkata

2015-03-06

A series of thirty three novel 6-(piperazin-1-yl)phenanthridine amide and sulphonamide analogues were synthesized, characterized and screened for their in vitro antimycobacterial activity against Mycobacterium tuberculosis (MTB) H37Rv strain. These compounds exhibited minimum inhibitory concentration (MIC) between 1.56 and ≥50 μg/mL. Out of these derivatives, few compounds 6l, 6r, 7b, 7f, 7g and 7k exhibited moderate activity (MIC = 6.25 μg/mL) and compounds 6b, 6e, 6k, 6n, 7h, 7i and 7n displayed good activity (MIC = 3.13 μg/mL), whereas compounds 6m, 6s and 7d exhibited excellent anti-tubercular activity (MIC = 1.56 μg/mL). In addition, MTT assay was accomplished on the active analogues of the series against mouse macrophage (RAW 264.7) cells to evaluate the toxicity profile of the newly synthesized compounds and selectivity index of the compounds was determined. Additionally, compounds 6b and 7d were docked to the ATPase domain of M. tuberculosis GyrB protein to know the interaction profile and structures of compounds 6b and 7d were further substantiated through single crystal XRD. Copyright © 2015 Elsevier Masson SAS. All rights reserved.

Enthalpies of melting of LnSF compounds (Ln = La, Ce, Pr, Nd, Sm)

NASA Astrophysics Data System (ADS)

Andreev, P. O.; Mikhalkina, O. G.; Andreev, O. V.; Elyshev, A. V.

2015-05-01

The melting temperatures and enthalpies of such congruently melting compounds as LaSF ( T m = 1713 ± 7 K, Δ H = 45.7 ± 4.6 kJ/mol), CeSF ( T m = 1683 ± 7 K, Δ H = 40.7 ± 4.1 kJ/mol), PrSF ( T m = 1661 ± 7 K, Δ H = 39.7 ± 4.0 kJ/mol), NdSF ( T m = 1654 ± 7 K, Δ H = 40.2 ± 4.0 kJ/mol), and SmSF ( T m = 1587 ± 7 K, Δ H = 36.1 ± 3.6 kJ/mol) are determined via synchronous thermal analysis. The tetrad effect is evident in the change of the melting temperatures and enthalpies of LnSF compounds (Ln = La, Ce, Pr, Nd, Sm) depending on r(Ln3+).

Design, synthesis and anticonvulsant activity of some new 6,8-halo-substituted-2h-[1,2,4]triazino[5,6-b]indole-3(5h)-one/-thione and 6,8-halo-substituted 5-methyl-2h-[1,2,4]triazino[5,6-b]indol-3(5h)-one/-thione

PubMed Central

Kumar, Rajeev; Singh, Tejendra; Singh, Hariram; Jain, Sandeep; Roy, R. K.

2014-01-01

A new series of 6,8-halo-substituted-2H-[1,2,4]triazino[5,6-b]indole-3(5H)-one/-thione and 6,8-halo-substituted 5-methyl-2H-[1,2,4]triazino[5,6-b]indol-3(5H)-one/-thione (5a-5l) were designed and synthesized keeping in view of the structural requirement of pharmacophore. The above compounds were characterized by thin layer chromatography and spectral analysis. Anticonvulsant activity of the synthesized compounds was evaluated by the maximal electroshock (MES) test. Neurotoxicity and CNS depressant effects were evaluated by the rotarod motor impairment and Porsolt’s force swim tests, respectively. A computational study was carried out, for calculation of pharmacophore pattern, prediction of pharmacokinetic properties and toxicity properties. The above study revealed that the compounds 8-chloro-2H-[1,2,4]triazino[5,6-b]indol-3(5H)-one (5e), 6,8-dibromo-2H-[1,2,4]triazino[5,6-b]indol-3(5H)-one (5i) and 6,8-dibromo-5-methyl-2H-[1,2,4]triazino[5,6-b]indol-3(5H)-one (5k) possess excellent anticonvulsant activity in the series with little CNS depressant effect and no neurotoxicity as compared to standard drugs phenytoin and carbamazepine. PMID:26417257

Synthesis and biological evaluation of some novel substituted 2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxamides

NASA Astrophysics Data System (ADS)

Jaismy Jacob, P.; Thomas, Anoop; Venkataraman, S.; Hareeshbabu, E.; Manju, S. L.

2017-11-01

A novel class of substituted 4-aryl-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxamide has been synthesized by simple, modified Hantzsch condensation reaction using N-arylacetoacetamides, aryl aldehydes and ammonia. Characterisation of the newly synthesized compounds was carried out by spectral analysis (IR, 1H NMR and Mass Spectroscopy). Antimicrobial activity against Staphylococcus aureus, Escherichia coli and Candida albicans and antiulcer activity by aspirin induced and pyloric ligation ulcer model was studied. Results revealed that most of the compounds exhibit significant antimicrobial activity along with antiulcer activity. The compound 6i 4-dimethylamino phenyl group at 4th position of 1,4-dihydropyridine had shown 65% ulcer protection at 10 mg/kg administration in male albino rats.

Synthesis of new substituted azetidinoyl and thiazolidinoyl-1,3,4-thiadiazino (6,5-b) indoles as promising anti-inflammatory agents.

PubMed

Bhati, Sudhir Kumar; Kumar, Ashok

2008-11-01

Various N-({5-[(arylmethylene)amino]-1,3,4-thiadiazol-2-yl}methyl) [1,3,4] thiadiazino[6,5-b]indol-3-amine (6a-6h), 2-aryl-3-{5-[([1,3,4] thiadiazino[6,5-b]indol-3-ylamino)methyl]-1,3,4-thiadiazol-2-yl}-1,3-thiazolidin-4-one (7a-7h), and 3-chloro-4-aryl-1-{5-[{[1,3,4]thiadiazino[6,5-b]indol-3-ylamino]methyl]-1,3,4-thiadiazol-2-yl}azetidin-2-one (8a-8h) have been synthesized in the present study. The structure of these newly synthesized compounds were confirmed by their analytical and spectral data. These compounds were also evaluated for their anti-inflammatory, ulcerogenic and analgesic activities. Compound 8g has shown most active anti-inflammatory and analgesic activities with better ulcerogenic activity than phenylbutazone, while this compound was found to be associated with lesser degree of anti-inflammatory and analgesic activities as compared to indomethacin.

Magnetic properties of the doubly ordered perovskite NaLnCoWO6 (Ln = Y, La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb) family

NASA Astrophysics Data System (ADS)

Zuo, Peng; Klein, Holger; Darie, Céline; Colin, Claire V.

2018-07-01

The focus of this study is on the magnetic properties of the very recently synthesized doubly ordered perovskite family NaLnCoWO6 (Ln = Y, La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, and Yb). Magnetic characterizations were performed by magnetic susceptibility vs. temperature, isothermal magnetization and heat capacity measurements. All these compounds have been determined as antiferromagnets with Néel temperatures from 4 K to 13.1 K. When the lanthanide is magnetic, additional transitions were observed below the Néel temperature which are attributed to the polarization of the magnetic Ln3+ sublattice by the ordered Co2+ one. Taking into account the magnetic ordering found in this study and the polar structure in the nine compounds NaLnCoWO6 (Ln = Y, Sm, Eu, Gd, Tb, Dy, Ho, Er, and Yb) reported before, these compounds can be classified as new Type I multiferroics.

Synthesis and anti-microbial activity of some 1- substituted amino-4,6-dimethyl-2-oxo-pyridine-3-carbonitrile derivatives.

PubMed

Khidre, Rizk E; Abu-Hashem, Ameen A; El-Shazly, Mohamed

2011-10-01

A new series of 1- substituted amino-4,6-dimethyl-2-oxo-pyridine-3-carbonitrile such as hydrazide hydrazones 3a-h; ethane-1,2-diaminopyridine 6; phthalimidopyridines 8a,b; hydrazides 10a,b; urea 11a and thiourea 11b were synthesized in a good to excellent yield in step efficient process, using 1-amino-4,6-dimethyl-2-oxo-1,2-dihydropyridine-3-carbonitrile (1) as a key intermediate. The antibacterial and antifungal activities of the synthesized compounds were evaluated. The obtained data indicated that the majority of the tested compounds exhibited both antibacterial and antifungal activities, particularly compounds 8a and 8b showed a comparable effect to a well known antibacterial and antifungal agents. Published by Elsevier Masson SAS.

Improvements in electrical and dielectric properties of substituted multiferroic LaMnO{sub 3} based nanostructures synthesized by co-precipitation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahmood, Azhar; Warsi, Muhammad Farooq, E-mail: Farooq.warsi@iub.edu.pk; Ashiq, Muhammad Naeem

2012-12-15

Graphical abstract: Display Omitted Highlights: ► Simultaneous double ion substitutions philosophy is introduced in LaMnO{sub 3}. ► La{sub 1−x}Gd{sub x}Mn{sub 1−y}Cr{sub y}O{sub 3} nanoparticles are not reported previously. ► La{sub 1−x}Gd{sub x}Mn{sub 1−y}Cr{sub y}O{sub 3} nanoparticles are synthesized by co-precipitation method. ► The 12 fold increase in resistivity of LaMnO{sub 3} nanostructures is observed. -- Abstract: A series of La{sub 1−x}Gd{sub x}Mn{sub 1−y}Cr{sub y}O{sub 3} nanoparticles (where x, y = 0, 0.25, 0.50, 0.75 and 1.0) has been synthesized by the chemical co-precipitation method, involving double ion substitution philosophy. The nanoparticles were characterized by thermo gravimetric analysis (TGA), X-ray fluorescencemore » spectrometry (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, vibrating sample magnetometer (VSM), DC electrical resistivity and dielectric measurements. The XRD and FTIR analysis confirmed the single orthorhombic phase and the crystallite size were found in the range of 16–34 nm. DC resistivity exhibited very interesting behavior which increased from 1.41 × 10{sup 8} to 16.35 ± 0.2 × 10{sup 8} Ω cm upon complete double ions replacement of La and Mn with Gd and Cr, respectively. This very high resistivity variation upon substitution definitely would open new avenues for applications of these materials in microwave devices and other related areas. The dielectric properties of these nanoparticles were also studied at room temperature in the range of 6 kHz to 5 MHz and the maximum dielectric behavior (ε′ = 2.86 × 10{sup 3}, tan δ = 5.41, ε″ = 15.5 × 10{sup 3}) was exhibited by La{sub 0.75}Gd{sub 0.25}Mn{sub 0.75}Cr{sub 0.25}O{sub 3} at 6 kHz. Hysteresis loops measurements showed that the synthesized nanomaterials are paramagnetic in nature at room temperature.« less

Synthesis and evaluation of 1,7-diheteroarylhepta-1,4,6-trien-3-ones as curcumin-based anticancer agents.

PubMed

Wang, Rubing; Zhang, Xiaojie; Chen, Chengsheng; Chen, Guanglin; Zhong, Qiu; Zhang, Qiang; Zheng, Shilong; Wang, Guangdi; Chen, Qiao-Hong

2016-03-03

Thirty (1E,4E,6E)-1,7-diaryl-1,4,6-heptatrien-3-ones, featuring a central linear trienone linker and two identical nitrogen-containing heteroaromatic rings, were designed and synthesized as curcumin-based anticancer agents on the basis of their structural similarity to the enol-tautomer of curcumin, in addition to taking advantage of the possibly enhanced pharmacokinetic profiles contributed by the basic nitrogen-containing heteroaromatic rings. Their cytotoxicity and antiproliferative activity were evaluated towards both androgen-dependent and androgen-independent prostate cancer cell lines, as well as HeLa human cervical cancer cells. Among them, the ten most potent analogues are 5- to 36-fold more potent than curcumin in inhibiting cancer cell proliferation. The acquired structure-activity relationship data indicate (i) that (1E,4E,6E)-1,7-diaryl-1,4,6-heptatrien-3-ones represent a potential scaffold for development of curcumin-based agents with substantially improved cytotoxicity and anti-proliferative effect; and (ii) 1-alkyl-1H-imidazol-2-yl and 1-alkyl-1H-benzo[d]imidazole-2-yl serve as optimal heteroaromatic rings for increased in vitro potency of this scaffold. Two of most potent compounds displayed no apparent cytotoxicity toward MCF-10A normal mammary epithelial cells at 1 μM concentration. Treatment of PC-3 prostate cancer cells with the most potent compound led to appreciable cell cycle arrest at a G1/G0 phase and cell apoptosis induction. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

Construction of New Coordination Polymers from 4’-(2,4-disulfophenyl)- 3,2’:6’3”-terpyridine: Polymorphism, pH-dependent syntheses, structures, and properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Li; Li, Chao-Jie; He, Jia-En

Nine new coordination compounds, namely, [Co(HDSPTP){sub 2}(H{sub 2}O){sub 4}]·4H{sub 2}O (H{sub 2}DSPTP=4’-(2,4-disulfophenyl)-3,2’:6’3”-terpyridine, 1 and 2), {[Ni(DSPTP)(H_2O)_4]·3H_2O}{sub n} (3), {[Cu(HDSPTP)_2(H_2O)_3]·8H_2O}{sub n} (4), {[Cu(HDSPTP)_2(H_2O)_3]·6H_2O}{sub n} (5), {[Cu(DSPTP)(H_2O)_2]·H_2O}{sub n} (6), {[Zn(DSPTP)(H_2O)_2]·2H_2O}{sub n} (7), {[Cd(DSPTP)(H_2O)_2]·2H_2O}{sub n} (8), and [Ag{sub 2}(DSPTP)(H{sub 2}O)]{sub n} (9), were constructed based on a new ligand containing both terpyridyl and sulfo groups. The reactions of H{sub 2}DSPTP with Co(NO{sub 3}){sub 2}.6H{sub 2}O resulted in two mononuclear complexes (compounds 1 and 2). They are polymorphisms that display different hydrogen bonding networks. They are selectively synthesized by altering the added alkalis. The reaction of H{sub 2}DSPTP with Ni(NO{sub 3}){sub 2}·6H{sub 2}O resultedmore » in a 1D “S-shaped” coordination chain (compound 3). The reactions of Cu(II) with H{sub 2}DSPTP at different pH value resulted in the following three compounds: two kinds of 1D chains obtained at pH 3.0 and 4.0 for compounds 4 and 5, respectively, and a 3D framework based on binuclear ring units with 4-connected sra topology (Compound 6). The reactions of H{sub 2}DSPTP with ds-block ions resulted in the following three compounds: a Zn(II) (compound 7) and a Cd(II) (compound 8) 3D frameworks with structures similar to that in compound 6, and a 3D framework based on tetranuclear Ag(I) SBUs with binodal (4,8)-connected flu type 3D framework topology. The structural diversity is mainly attributed to the rich coordination modes (from monodentate to µ{sub 7}-mode) and conformations (cis–cis and cis–trans) of HDSPTP{sup −}/DSPTP{sup 2−} ligands and the metal center and can be controllable synthesized by altering the alkalis, and pH value. Thermal stability of all compounds was performed, and the thermal behaviors of compounds 6 and 8 were further explored by PXRD. Compound 6

Hydrogen bonded supra-molecular framework in inorganic-organic hybrid compounds: Syntheses, structures, and photoluminescent properties

NASA Astrophysics Data System (ADS)

Yan, Li; Liu, Wei; Li, Chuanbi; Wang, Yifei; Ma, Li; Dong, Qinqin

2013-03-01

Two novel compounds constructed from aromatic acid and N-Heterocyclic ligands have been synthesized by hydrothermal reaction: [Cd(mip)(1,8-NDC)(H2O)]2 (1) [mip = 2-(3-methoxyphenyl)-1H-imidazo[4,5-f][1,10]phenanthroline, 1,8-NDC = naphthalene-1,8-dicarboxylic acid] and Cd(mip)2(NTC)2 (2) [NTC = nicotinic acid]. Compounds 1 and 2 are characterized by elemental analysis, IR, single crystal X-ray diffraction and thermogravimetric analysis (TGA). Single-crystal X-ray investigation reveals that compounds 1-2 are 0 dimensional (0D) structures, and the existence of hydrogen bonds and π-π interactions lead the 0D to 2D novel framework. Hydrogen bonds and π-π interactions are powerful non-covalent intermolecular interactions for directing supra-molecular architectures. TG analysis shows clear courses of weight loss, which corresponds to the decomposition of different ligands. At room temperature, compound 1 exhibits emission at 449 nm upon excitation at 325 nm, and compound 2 shows a strong emission at 656 nm upon excitation at 350 nm. Fluorescent spectrum displays that compounds 1 and 2 are potential luminescent materials.

6-(1-Benzyl-1H-pyrrol-2-yl)-2,4-dioxo-5-hexenoic acids as dual inhibitors of recombinant HIV-1 integrase and ribonuclease H, synthesized by a parallel synthesis approach.

PubMed

Costi, Roberta; Métifiot, Mathieu; Esposito, Francesca; Cuzzucoli Crucitti, Giuliana; Pescatori, Luca; Messore, Antonella; Scipione, Luigi; Tortorella, Silvano; Zinzula, Luca; Novellino, Ettore; Pommier, Yves; Tramontano, Enzo; Marchand, Christophe; Di Santo, Roberto

2013-11-14

The increasing efficiency of HAART has helped to transform HIV/AIDS into a chronic disease. Still, resistance and drug-drug interactions warrant the development of new anti-HIV agents. We previously discovered hit 6, active against HIV-1 replication and targeting RNase H in vitro. Because of its diketo-acid moiety, we speculated that this chemotype could serve to develop dual inhibitors of both RNase H and integrase. Here, we describe a new series of 1-benzyl-pyrrolyl diketohexenoic derivatives, 7a-y and 8a-y, synthesized following a parallel solution-phase approach. Those 50 analogues have been tested on recombinant enzymes (RNase H and integrase) and in cell-based assays. Approximately half (22) exibited inhibition of HIV replication. Compounds 7b, 7u, and 8g were the most active against the RNase H activity of reverse-transcriptase, with IC50 values of 3, 3, and 2.5 μM, respectively. Compound 8g was also the most potent integrase inhibitor with an IC50 value of 26 nM.

Nanoscale modulations in (KLa)(CaW)O{sub 6} and (NaLa)(CaW)O{sub 6}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Licurse, Mark W., E-mail: mlicurse@seas.upenn.edu; Borisevich, Albina Y., E-mail: albinab@ornl.gov; Davies, Peter K., E-mail: davies@seas.upenn.edu

2012-07-15

Complex nanoscale modulations are identified in two new A-site ordered perovskites, (KLa)(CaW)O{sub 6} and (NaLa)(CaW)O{sub 6}. In (KLa)(CaW)O{sub 6}, selected-area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM) show an incommensurate nanocheckerboard modulation with {approx}9.4 Multiplication-Sign 9.4a{sub p} periodicity (a{sub p} Almost-Equal-To 4 A for the cubic perovskite aristotype). For (NaLa)(CaW)O{sub 6} a one-dimensional modulation is observed with a {approx}16(1 1 0)a{sub p} repeat; the Left-Pointing-Angle-Bracket 1 1 0 Right-Pointing-Angle-Bracket orientation of the nanostripes is different from the Left-Pointing-Angle-Bracket 1 0 0 Right-Pointing-Angle-Bracket stripes observed in other mixed A-site systems. Studies using high temperature x-ray diffraction suggest the formationmore » of the complex modulations is associated with small deviations from the ideal 1:1:1:1 stoichiometry of the (A{sup +}La{sup 3+})(CaW)O{sub 6} phases. Z-contrast images acquired on an aberration-corrected microscope provide evidence for deviations from stoichiometry with a {approx}1:15 periodic arrangement of La{sub 4/3}(CaW)O{sub 6}:(NaLa)(CaW)O{sub 6} nano-phases. - Graphical abstract: Complex nanoscale modulations are identified in two new A-site ordered perovskites, (KLa)(CaW)O{sub 6} and (NaLa)(CaW)O{sub 6}. In (KLa)(CaW)O{sub 6}, selected-area electron diffraction and high-resolution transmission electron microscopy show a two-dimensional, nanocheckerboard modulation. For (NaLa)(CaW)O{sub 6} a one-dimensional modulation is observed; the Left-Pointing-Angle-Bracket 1 1 0 Right-Pointing-Angle-Bracket orientation of the nanostripes is different from the Left-Pointing-Angle-Bracket 1 0 0 Right-Pointing-Angle-Bracket stripes observed in other mixed A-site systems. Highlights: Black-Right-Pointing-Pointer Two new A-site ordered perovskites were synthesized, (KLa)(CaW)O{sub 6} and (NaLa)(CaW)O{sub 6}. Black

Construction of New Coordination Polymers from 4'-(2,4-disulfophenyl)- 3,2':6'3"-terpyridine: Polymorphism, pH-dependent syntheses, structures, and properties

NASA Astrophysics Data System (ADS)

Zhang, Li; Li, Chao-Jie; He, Jia-En; Chen, Yin-Yu; Zheng, Sheng-Run; Fan, Jun; Zhang, Wei-Guang

2016-01-01

Nine new coordination compounds, namely, [Co(HDSPTP)2(H2O)4]·4H2O (H2DSPTP=4'-(2,4-disulfophenyl)-3,2':6'3"-terpyridine, 1 and 2), {[Ni(DSPTP)(H2O)4]·3H2O}n (3), {[Cu(HDSPTP)2(H2O)3]·8H2O}n (4), {[Cu(HDSPTP)2(H2O)3]·6H2O}n (5), {[Cu(DSPTP)(H2O)2]·H2O}n (6), {[Zn(DSPTP)(H2O)2]·2H2O}n (7), {[Cd(DSPTP)(H2O)2]·2H2O}n (8), and [Ag2(DSPTP)(H2O)]n (9), were constructed based on a new ligand containing both terpyridyl and sulfo groups. The reactions of H2DSPTP with Co(NO3)2.6H2O resulted in two mononuclear complexes (compounds 1 and 2). They are polymorphisms that display different hydrogen bonding networks. They are selectively synthesized by altering the added alkalis. The reaction of H2DSPTP with Ni(NO3)2·6H2O resulted in a 1D "S-shaped" coordination chain (compound 3). The reactions of Cu(II) with H2DSPTP at different pH value resulted in the following three compounds: two kinds of 1D chains obtained at pH 3.0 and 4.0 for compounds 4 and 5, respectively, and a 3D framework based on binuclear ring units with 4-connected sra topology (Compound 6). The reactions of H2DSPTP with ds-block ions resulted in the following three compounds: a Zn(II) (compound 7) and a Cd(II) (compound 8) 3D frameworks with structures similar to that in compound 6, and a 3D framework based on tetranuclear Ag(I) SBUs with binodal (4,8)-connected flu type 3D framework topology. The structural diversity is mainly attributed to the rich coordination modes (from monodentate to μ7-mode) and conformations (cis-cis and cis-trans) of HDSPTP-/DSPTP2- ligands and the metal center and can be controllable synthesized by altering the alkalis, and pH value. Thermal stability of all compounds was performed, and the thermal behaviors of compounds 6 and 8 were further explored by PXRD. Compound 6 exhibits low thermal stability and undergo a crystalline-crystalline-amorphous phase transition as temperature increases from 25 °C to 200 °C, and show amorphous-crystalline phase transition when rehydrated

Fabrication of aligned porous LaNi0.6Fe0.4O3 perovskite by water based freeze casting

NASA Astrophysics Data System (ADS)

Soltani, Niloofar; Martínez-Bautista, Rubén; Bahrami, Amin; Huerta Arcos, Lázaro; Cassir, Michel; Chávez Carvayar, José

2018-05-01

A novel porous cathode of LaNi0.6Fe0.4O3 perovskite with aligned porosities was engineered for solid oxide fuel cells. LaNi0.6Fe0.4O3 was produced through metal nitrate and acid citric combustion method and calcined at different temperatures. The synthesized LNF at 600 °C shows specific surface area (SBET) of 24.4 m2 g-1 and an average pore size of 12.2 nm. The chemical composition and structure of LaNi0.6Fe0.4O3 synthesized at temperature 600-1400 °C, were analyzed by XRD, XPS and HRTEM. SEM observations of freeze cast nano-sized LNF showed the vertically aligned hexagonal walls. These walls contain a great value of fine pores which accelerate the gas transportation.

5-(Furan-2-yl)-4-(3,4,5-trimethoxyphenyl)-3H-1,2-dithiol-3-one oxime (6f), a new synthetic compound, causes human fibrosarcoma HT-1080 cell apoptosis by disrupting tubulin polymerisation and inducing G2/M arrest.

PubMed

Zuo, Daiying; Pang, Lili; Shen, Jiwei; Guan, Qi; Bai, Zhaoshi; Zhang, Huijuan; Li, Yao; Lu, Guodong; Zhang, Weige; Wu, Yingliang

2017-06-01

In the current study, we synthesized a series of new compounds targeting tubulin and tested their anti-proliferative activities. Among these new synthetic com-pounds, 5-(furan-2-yl)-4-(3,4,5-trimethoxyphenyl)-3H-1,2-dithiol-3-one oxime (6f) exhibited significant anti-proliferative activity against different human cancer cell lines including human gastric adenocarcinoma SGC-7901, human non-small cell lung cancer A549, and human fibrosarcoma HT-1080. As a result, 6f was selected to further test the sensitivity to different cancer cell lines including human cervical cancer cell line HeLa, human breast cancer cell line MCF-7, non-small cell lung cancer cell line A549, human liver carcinoma cell line HepG-2, human oral squamous cell carcinoma cell lines KB, SGC-7901 and HT-1080. Among these cell lines, HT-1080 and HeLa are the most sensitive. Therefore, HT-1080 was selected to further explore the properties of anti-proliferative activity and the underlying mechanisms. Our data proved that 6f exhibited strong anti-proliferative effects against HT-1080 cells in a time- and dose-dependent manner. We showed that the growth inhibitory effect of 6f in HT-1080 cells was related with microtubule depolymerisation. Molecular docking studies revealed that 6f interacted and bound efficiently with the colchicine-binding site of tubulin. In addition, 6f treatment induced G2/M cell cycle arrest dose-dependently and subsequently induced cell apoptosis. Western blot study indicated that upregulation of cyclin B1 and p-cdc2 was related with G2/M arrest. 6f-induced cell apoptosis was associated with both mitochondrial and death receptor pathway. In conclusion, our data showed that 6f, among the newly synthetic compounds, exhibited highest anti-proliferative activity by disrupting the microtubule polymerisation, causing G2/M arrest and subsequently inducing cell apoptosis in HT-1080 cells. Hence, 6f is a promising microtubule depolymerising agent for the treatment of various cancers

Molecular structure, quantum mechanical calculation and radical scavenging activities of (E)-4,6-dibromo-2-[(3,5-dimethylphenylimino)methyl]-3-methoxyphenol and (E)-4,6-dibromo-2-[(2,6-dimethylphenylimino)methyl]-3-methoxyphenol compounds.

PubMed

Alaşalvar, Can; Soylu, Mustafa Serkan; Güder, Aytaç; Albayrak, Çiğdem; Apaydın, Gökhan; Dilek, Nefise

2014-09-15

In this study, (E)-4,6-dibromo-2-[(3,5-dimethylphenylimino)methyl]-3-methoxyphenol and (E)-4,6-dibromo-2-[(2,6-dimethylphenylimino)methyl]-3-methoxyphenol compounds have been synthesized and characterized by using X-ray crystallographic method, FT-IR and Density functional method. The molecular geometry, vibrational frequencies of the title compounds in the ground state have been calculated by using B3LYP with the 6-31G(d,p) basis set. The tautomeric form of the compounds has been demonstrated by using single crystal X-ray method, FT-IR spectrometer and DFT method. In addition, HOMO-LUMO energy gap, molecular electrostatic potential map and NBO analysis of the compounds are performed at B3LYP/6-31G(d,p) level. It may be remarked that the free radical scavenging activities of the title compounds were assessed using DPPH, DMPD+, and ABTS+ assays. The obtained results show that especially compound 2 has effective DPPH (SC50 1.52±0.14 μg/mL), DMPD+ (SC50 1.22±0.21 μg/mL), and ABTS+ (SC50 3.32±0.17 μg/mL) scavenging activities compared with standards (BHA, rutin, and trolox). Copyright © 2014 Elsevier B.V. All rights reserved.

Syntheses, structures and luminescence for zinc coordination polymers based on a multifunctional 4‧-(3-carboxyphenyl)- 3,2‧:6‧,3″-terpyridine ligand

NASA Astrophysics Data System (ADS)

Cheng, Yue; Yang, Meng-Lin; Hu, Huai-Ming; Xu, Bing; Wang, Xiaofang; Xue, Ganglin

2016-07-01

Six new coordination polymers, [ZnLCl]n(1), [ZnL2]n·2nH2O (2), [Zn2L(o-bdc)(OH)]n·0.5nH2O (3), [Zn2L(m-bdc)(OH)]n·nH2O (4), [Zn2L2(p-bdc) (H2O)2]n·nH2O (5), [Zn2L(1,2,4-btc)(H2O)]n(6), (HL=4‧-(3-carboxyphenyl)- 3,2‧:6‧,3″-terpyridine, H2(o-bdc)= benzene-1,2-dicarboxylic acid, H2(m-bdc)= benzene-1,3-dicarboxylic acid, H2(p-bdc)= benzene-1,4-dicarboxylic acid, H3(1,2,4-btc)= benzene-1,2,4-tricarboxylic acid) have been synthesized under the hydrothermal conditions. Compound 1 displays a 3-connected 2D network structure with point symbol of {82.10}. Compound 2 exhibits 1D infinite loop chain structure. Compound 3 possesses a (3,8)-connected 3D framework composed of tetranuclear units with point symbol of {43}2{46.618.84}. Compound 4 features a typical 2D hcb network based on tetranuclear zinc(II) units with point symbol of {44.62}. Compound 5 presents a classical two-fold penetration sql network with point symbol of {63}. Compound 6 can be seen as a (3,3,6)-connected 3D net with point symbol of {42.64.89}{42.6}{63}. The thermal stability and luminescent properties of compounds 1-6 in the solid state are discussed in detail.

Structural characterization, electrical conductivity and open circuit voltage studies of the nanocrystalline La10Si6O27 electrolyte material for SOFCs

NASA Astrophysics Data System (ADS)

Jena, Paramananda; Jayasubramaniyan, S.; Patro, P. K.; Lenka, R. K.; Sinha, Amit; Muralidharan, P.; Srinadhu, E. S.; Satyanarayana, N.

2018-02-01

Nanocrystalline La10Si6O27 apatite-type sample was synthesized by the co-precipitation method. Thermal behavior, phase, structure, morphology and elemental composition of La, O and Si of the synthesized La10Si6O27 sample were investigated through TG/DTA, XRD, FTIR, Raman spectroscopy and SEM-EDX measurements respectively. Formation of phase purity of the nanocrystalline La10Si6O27 sample was confirmed by analysing the measured X-ray powder diffraction (XRD) pattern using Rietveld refinement and the calculated average crystallite size of the La10Si6O27 sample was found to be 33 nm. The electrical conductivity of the sintered La10Si6O27 pellet was investigated as a function of temperature ranging from 200 to 800 °C under air and it was found to be 1.92 × 10-3 S cm-1 at 800 °C. The chemical stability of La10Si6O27 powder under oxidizing and reducing atmospheres was confirmed from the analysis of the measured XRD pattern and Raman spectral results. Open circuit potential of a button cell, made up of the La10Si6O27 sample, was tested up to 800 °C with both oxygen and hydrogen at opposite sides of the cell and was found to 1 V. Hence, the results demonstrate that La10Si6O27 could be a promising solid electrolyte material for the solid oxide fuel cell (SOFC) applications.

Temperature-controlled two new Co(II) compounds with distinct topological networks: Syntheses, crystal structures and catalytic properties

NASA Astrophysics Data System (ADS)

Meng, Qing-Hua; Long, Xu; Liu, Jing-Li; Zhang, Shuan; Zhang, Guang-Hui

2018-04-01

Two new Co(II) coordination compounds, namely [Co2(bptc)(bpp)2]n (1) and [Co(bptc)0.5(bpp)]n (2) (H4bptc = biphenyl-3,3‧,5,5‧-tetracarboxylic acid, bpp = 1,3-di(4-pyridyl)propane), have been hydrothermally synthesized from the same reactants via tuning the reaction temperature. Single crystal X-ray diffraction analyses revealed that both 1 and 2 feature 2D sheet motifs. Topological analyses revealed that compounds 1 and 2 show distinct topological networks. Under the weak Van der Waals interactions, the 2D sheet motifs of compounds 1 and 2 are further packed into 2D→3D interdigitated supramolecular frameworks. Moreover, the two Co(II) compounds show high catalytic activities for degradation of methyl orange (MO) in a Fenten-like process.

Two isomeric lead(II) carboxylate-phosphonates: syntheses, crystal structures and characterizations

NASA Astrophysics Data System (ADS)

Lei, Chong; Mao, Jiang-Gao; Sun, Yan-Qiong

2004-07-01

Two isomeric layered lead(II) carboxylate-phosphonates of N-(phosphonomethyl)- N-methyl glycine ([MeN(CH 2CO 2H)(CH 2PO 3H 2)]=H 3L), namely, monoclinic Pb 3L 2·H 2O 1 and triclinic Pb 3L 2·H 2O 2, have been synthesized and structurally determined. Compound 1 synthesized by hydrothermal reaction at 150°C is monoclinic, space group C2/ c with a=19.9872(6), b=11.9333(1) and c=15.8399(4) Å, β=110.432(3)°, V=3540.3(1) Å 3, and Z=8. The structure of compound 1 features a <400> layer in which the lead(II) ions are bridged by both phosphonate and carboxylate groups. The lattice water molecules are located between the layers, forming hydrogen bonds with the non-coordinated carboxylate oxygen atoms. Compound 2 with a same empirical formula as compound 1 was synthesized by hydrothermal reaction at 170°C. It has a different layer structure from that of compound 1 due to the adoption of a different coordination mode for the ligand. It crystallizes in the triclinic system, space group P 1¯ with cell parameters of a=7.1370(6), b=11.522(1), c=11.950(1) Å, α=110.280(2), β=91.625(2), γ=95.614(2)°, V=915.3(1) Å 3 and Z=2. The structure of compound 2 features a <020> metal carboxylate-phosphonate double layer built from 1D lead(II) carboxylate chains interconnected with 1D lead(II) phosphonate double chains. XRD powder patterns of compounds 1 and 2 indicate that each compound exists as a single phase.

6. Photocopy of pencil drawing (on file at La Grande ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

6. Photocopy of pencil drawing (on file at La Grande District Office, La Grande, Oregon) USDA Forest Service, 1939 CIRCULATION PLAN - Union Ranger District Compound, Fronting State Highway 203, at West edge of Union, Union, Union County, OR

The effects of Tb substitution for La on the magnetic properties of LaFe11.5Si1.5 compound

NASA Astrophysics Data System (ADS)

Imam, H.; Zhang, H. G.; Xu, L.; Zhao, J. L.; Gao, X. X.; Yue, M.

2018-05-01

The structural and magnetic properties of La1-yTbyFe11.5Si1.5 compounds have been investigated. The substituted 5 percent of Tb has remarkably increased the maximum entropy change (-ΔSM) to a value of 25.2 J/kg·K. However, a further increase of Tb leads to a monotonous decrease in the entropy change, mainly due to phase separation. The Tb substitution also can lower the thermal and magnetic hysteresis loss of the system. Another feature of this replacement is that, with Tb content higher than 10 percent, the Curie temperature (TC) starts to increase and reaches 197 K when 30 percent of La is substituted. These results indicate that La1-yTbyFe11.5Si1.5 may be a promising candidate for magnetic refrigeration material in certain temperature range.

Cyclic guanidines: synthesis and antiplatelet activity of 4,6,7,8-tetrahydro-1H-imidazo[1,2-a]pyrazolo[3,4-d]pyrimidin-7-ones and 1,4,6,7,8,9-hexahydropyrazolo [3',4':4,5]pyrimido[2,1-c] [1,2,4]triazin-7-ones.

PubMed

Ferroni, R; Simoni, D; Orlandini, P; Bardi, A; Franze, G P; Guarneri, M

1990-12-01

A series of 4,6,7,8-tetrahydro-1H-imidazo[1,2-a]pyrazolo [3,4-d]pyrimidin-7-ones (1b-n) and 1,4,6,7,8,9-hexahydropyrazolo [3',4':4,5]pyrimido [2,1-c][1,2,4]triazin-7-ones (2a-d) has been synthesized. In view of their potential anti-aggregating activity the compounds were tested in vitro for inhibitory activity towards ADP- and collagen-induced aggregation of human platelets. Among the compounds studied, 8-benzyl-1-(2,5-dichlorophenyl)-4,6,7,8-tetrahydro-1H-imidazo [1,2-a]pyrazolo[3,4-d]pyrimidin-7-one (1n) exhibited the most favorable activity. The 2,5-dichlorophenyl side chain is an important lipophilic and/or steric pharmacophore.

6. Photocopy of architectural blueprint (on file at La Grande ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

6. Photocopy of architectural blueprint (on file at La Grande District Office, La Grande, Oregon) USDA Forest Service RANGERS RESIDENCE - Union Ranger Distric Compound, Rangers Residence, Fronting State Highway 203, at West edge of Union, Union, Union County, OR

Structure determination of {alpha}-La{sub 6}W{sub 2}O{sub 15}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chambrier, M-H., E-mail: marie-helene.chambier.etu@univ-lemans.f; Ibberson, R.M.; Goutenoire, F., E-mail: francois.goutenoire@univ-lemans.f

2010-06-15

The structure of the high temperature alpha form of La{sub 6}W{sub 2}O{sub 15} has been determined ab-initio from high temperature laboratory X-ray and neutron time-of-flight data. This tungstate crystallizes in the non-centrosymmetric orthorhombic space group (No. 20) C222{sub 1}, with Z=2, a=12.6250(2) A, b=9.1875(1) A, c=5.9688(1) A. The structure comprises [O{sub 2}La{sub 3}] infinite ribbons and is better described by the structural formula [O{sub 2}La{sub 3}]{sub 2}[WO{sub 5.5}]{sub 2}. Using this description we can understand the strong structural similarity of the present compound with compounds of the general composition BiM{sub 2}AO{sub 6} (M=Cu, Mg, Zn, Mn, Cd, Ca, Pb; A=P,more » As, V) described as [O{sub 2}M{sub 2}Bi][AO{sub 4}]. The [WO{sub 5.5}] entity implies oxygen disorder in the material. - Graphical abstract: Projection of the polyhedra around the tungsten atom. Atoms labelled in grey are occupied at 50%. Short oxygen-oxygen distances are marked. The polyhedra represents WO{sub 5.5} that is related to the structural unit W{sub 2}O{sub 11} unit. Alpha-La{sub 6}W{sub 2}O{sub 15} could be described as [O{sub 2}La{sub 3}]{sub 2}[WO{sub 5.5}]{sub 2}.« less

A Simple and Efficient Synthesis of 4-Arylacridinediones and 6-Aryldiindeno[1,2-b:2,1-e]pyridinediones using CuI Nanoparticles as Catalyst under Solvent-Free Conditions.

PubMed

Abdolmohammadi, Shahrzad; Dahi-Azar, Saman; Mohammadnejad, Mahdieh; Hosseinian, Akram

2017-01-01

The importance of acridine core structure and other heterocycles containing its framework is well known, as they are found in numerous compounds with a variety of biological effects. Pyridine is also an important solvent and heterocyclic nucleus for the design and synthesis of novel molecules with biological properties. It occurs in several natural compounds which are used as a precursor in agrochemicals and pharmaceuticals. The utility of nanostructured metal salts because of their small size and high surface area as catalysts in organic synthesis has drawn special attention due to their better properties such as slower reaction rate, reusability of the catalyst, and higher yields of products compared to the bulk size. Nanosized copper iodide is one reusable Lewis acid catalyst which has revealed several catalytic activities for the synthesis of organic compounds and others. As part of our recent study to develop heterocyclic syntheses using nanostructured catalysts, we now report an efficient and clean synthetic route to 4-arylacridinediones and 6-aryldiindeno[1,2-b:2,1-e]pyridinediones via a condensation reaction catalyzed by CuI nanoparticles under solvent-free conditions. The present work deals with the condensation reaction of aromatic aldehydes, ammonium acetate and active methylene compounds comprising dimedone or 1,3- indanedione in the presence of a catalytic amount of the synthesized CuI nanoparticles could be applied for the solvent-free preparation of 4-arylacridinediones and 6-aryldiindeno[1,2-b:2,1- e]pyridinediones at 70 °C within 60 min. A series of 9-aryl-3,3,6,6-tetramethyl-3,4,6,7,9,10-hexahydro-1,8(2H,5H)-acridinediones and 6-aryldiindeno[1,2-b:2,1-e]pyridine-5,7-diones were synthesized in high to excellent yields via a simple one-pot three-component coupling reaction using the synthesized CuI nanoparticles as an efficient and recyclable catalyst. All synthesized compounds were well characterized by their satisfactory elemental analyses, IR, 1

Electrical conductivity and thermoelectric power of La1- x Li x CoO3-δ (0 ≤ x ≤ 0.1) oxides

NASA Astrophysics Data System (ADS)

Vecherskii, S. I.; Konopel'ko, M. A.; Batalov, N. N.; Antonov, B. D.; Reznitskikh, O. G.; Yaroslavtseva, T. V.

2016-12-01

The influence of the concentration of lithium ions on the phase composition, the electrical conductivity, and the thermoelectric power of La1- x Li x CoO3-δ (0 ≤ x ≤ 0.1) oxides synthesized by the ceramic method has been investigated. It has been found that the region of the existence of perovskite-type La1- x Li x CoO3-δ solid solutions does not exceed x = 0.05. The doping with lithium leads to an increase in the electrical conductivity of single-phase samples in comparison with that of the LaCoO3 compound. As the temperature increases from 300 to 400 K, the thermoelectric power of the LaCoO3 compound increases from the negative to positive values and then decreases, but remains positive in the temperature range from 400 to 1020 K. The thermoelectric power of the other samples has a positive sign. The results obtained have been discussed based on the models of the electron density of states in LaCoO3 and La1- x Sr x CoO3-δ, proposed in the studies of Señarís-Rodríguez and Goodenough, as well as in the framework of the theory of non-crystalline materials, developed by Mott.

6. Photocopy of architectural blueprint (on file at La Grande ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

6. Photocopy of architectural blueprint (on file at La Grande District Office, La Grande, Oregon) USDA Forest Service, 1936 THREE-ROOM OFFICE (SHEET 4) - Union Ranger District Compound, Office, Fronting State Highway 203, at West edge of Union, Union, Union County, OR

A new route for the synthesis of submicron-sized LaB{sub 6}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lihong, Bao; Wurentuya,; Wei, Wei

Submicron crystalline LaB{sub 6} has been successfully synthesized by a solid-state reaction of La{sub 2}O{sub 3} with NaBH{sub 4} at 1200 °C. The effects of reaction temperature on the crystal structure, grain size and morphology were investigated by X-ray diffraction, scanning electron microscope and transmission electron microscope. It is found that when the reaction temperature is in the range of 1000–1100 °C, there are ultrafine nanoparticles and nanocrystals that coexist. When the reaction temperature elevated to 1200 °C, the grain morphology transformed from ultrafine nanoparticle to submicron crystals completely. High resolution transmission electron microscope images fully confirm the formation ofmore » LaB{sub 6} cubic structure. - Highlights: • Single-phased LaB{sub 6} have been synthesized by a solid-state reaction in a continuous evacuating process. • The reaction temperature has a important effect on the phase composition. • The grain size increase from nano-size to submicron with increasing reaction temperature.« less

Inhibitory activity of synthesized acetylated Procyanidin B1 analogs against HeLa S3 cells proliferation.

PubMed

Okamoto, Syuhei; Ishihara, Sayaka; Okamoto, Taisuke; Doi, Syoma; Harui, Kota; Higashino, Yusuke; Kawasaki, Takashi; Nakajima, Noriyuki; Saito, Akiko

2014-02-04

Proanthocyanidins, also known as condensed tannins and/or oligomeric flavonoids, occur in many edible plants and have various interesting biological activities. Previously, we reported a synthetic method for the preparation of various procyanidins in pure form and described their biological activities. Here, we describe the synthesis of procyanidin B1 acetylated analogs and discuss their inhibition activities against HeLa S3 cell proliferation. Surprisingly, the lower-unit acetylated procyanidin B1 strongly inhibited the proliferation of HeLa S3 cells. This molecule showed much stronger inhibitory activity than did epigallocatechin-3-O-gallate (EGCG), green tea polyphenol, and dimeric compounds that included EGCG as a unit. This result suggests that the phenolic hydroxyl groups of the upper-units in flavan-3-ols are important for their inhibitory activity against cancer cell proliferation and that a hydrophobic lower unit dimer enhances this activity.

[H{sub 2}en]{sub 2}{l_brace}La{sub 2}M(SO{sub 4}){sub 6}(H{sub 2}O){sub 2}{r_brace} (M=Co, Ni): First organically templated 3d-4f mixed metal sulfates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yuan Yanping; Wang Ruiyao; Kong Deyuan

2005-06-15

The first organically templated 3d-4f mixed metal sulfates, [H{sub 2}en]{sub 2}{l_brace}La{sub 2}M(SO{sub 4}){sub 6}(H{sub 2}O){sub 2}{r_brace} (M=Co 1, Ni 2) have been synthesized and structurally determined from non-merohedrally twinned crystals. The two compounds are isostructural and their structures feature a three-dimensional anionic network formed by the lanthanum(III) and nickel(II) ions bridged by sulfate anions. The La(III) ions in both compounds are 10-coordinated by four sulfate anions in bidentate chelating fashion, and two sulfate anions in a unidentate fashion. The transition metal(II) ion is octahedrally coordinated by six oxygens from four sulfate anions and two aqua ligands. The doubly protonated enthylenediaminemore » cations are located at the tunnels formed by 8-membered rings (four La and four sulfate anions)« less

Synthesis and Antimicrobial Activity of 6-Thioxo-6,7-dihydro-2H-[1,2,4]triazino[2,3-c]-quinazolin-2-one Derivatives

PubMed Central

Nosulenko, Inna S.; Voskoboynik, Olexii Yu.; Berest, Galina G.; Safronyuk, Sergiy L.; Kovalenko, Sergiy I.; Kamyshnyi, Oleksandr M.; Polishchuk, Nataliya M.; Sinyak, Raisa S.; Katsev, Andrey V.

2014-01-01

Abstract Potassium 8-R1-9-R2-10-R3-3-R-2-oxo-2H-[1,2,4]triazino[2,3-c]quinazoline-6-thiolates 2.1–2.26 were synthesized via cyclocondensation of 6-R-3-(3-R1-4-R2-5-R3-aminophenyl)-1,2,4-triazin-5-ones 1.1–1.26 with carbon disulfide, potassium hydroxide, and ethanol or with potassium O-ethyl dithiocarbonate in 2-propanol. The corresponding thiones 3.1–3.26 were obtained by treatment of 2.1–2.26 with hydrochloric acid. It was found that the nature of the substituents in positions 3, 4, and 5 of the corresponding 6-R-3-(3-R1-4-R2-5-R3-aminophenyl)-1,2,4-triazin-5-ones were affected on the terms of the reaction. The structures of compounds were proven by a complex of physicochemical methods (1H, 13C NMR, LC–MS, and EI-MS). The results of the antibacterial and antifungal activity assay allowed the determination of the high sensitivity of Staphylococcus aureus ATCC 25923 (MIC 6.25–100 μg/mL, MBC 12.5–200 μg/mL) to the synthesized compounds. PMID:25853063

Involvement of S6K1 in mitochondria function and structure in HeLa cells.

PubMed

Park, Jisoo; Tran, Quangdon; Mun, Kisun; Masuda, Kouhei; Kwon, So Hee; Kim, Seon-Hwan; Kim, Dong-Hoon; Thomas, George; Park, Jongsun

2016-12-01

The major biological function of mitochondria is to generate cellular energy through oxidative phosphorylation. Apart from cellular respiration, mitochondria also play a key role in signaling processes, including aging and cancer metabolism. It has been shown that S6K1-knockout mice are resistant to obesity due to enhanced beta-oxidation, with an increased number of large mitochondria. Therefore, in this report, the possible involvement of S6K1 in regulating mitochondria dynamics and function has been investigated in stable lenti-shS6K1-HeLa cells. Interestingly, S6K1-stably depleted HeLa cells showed phenotypical changes in mitochondria morphology. This observation was further confirmed by detailed image analysis of mitochondria shape. Corresponding molecular changes were also observed in these cells, such as the induction of mitochondrial fission proteins (Drp1 and Fis1). Oxygen consumption is elevated in S6K1-depeleted HeLa cells and FL5.12 cells. In addition, S6K1 depletion leads to enhancement of ATP production in cytoplasm and mitochondria. However, the relative ratio of mitochondrial ATP to cytoplasmic ATP is actually decreased in lenti-shS6K1-HeLa cells compared to control cells. Lastly, induction of mitophagy was found in lenti-shS6K1-HeLa cells with corresponding changes of mitochondria shape on electron microscope analysis. Taken together, our results indicate that S6K1 is involved in the regulation of mitochondria morphology and function in HeLa cells. This study will provide novel insights into S6K1 function in mitochondria-mediated cellular signaling. Copyright © 2016 Elsevier Inc. All rights reserved.

Synthesis and antiproliferative activity of 6-phenylaminopurines.

PubMed

Canela, María-Dolores; Liekens, Sandra; Camarasa, María-José; Priego, Eva María; Pérez-Pérez, María-Jesús

2014-11-24

A series of novel 6-phenylaminopurines have been efficiently synthesized in 3 steps exploring different groups at positions 2, 8 and 9 of the purine ring and at the exocyclic nitrogen atom at position 6. Among the newly described purines, five compounds showed antiproliferative activity with IC50 values below 10 μM, the tetrahydroquinoline derivative at position 6 of phenylaminopurine being the most active of the series in the six cell lines tested. Moreover, the compounds induced G2/M phase arrest in human cervical carcinoma HeLa cells as reported for tubulin depolymerizing agents. Copyright © 2014 Elsevier Masson SAS. All rights reserved.

Positive magnetoresistance of single-crystal bilayer manganites (La{sub 1−z}Nd{sub z}){sub 1.4}Sr{sub 1.6}Mn{sub 2}O{sub 7} (z = 0, 0.1)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shaykhutdinov, K. A.; Petrov, M. I.; Terent'ev, K. I.

2015-04-28

We investigate magnetoresistance, ρ{sub c}, of single-crystal bilayer lanthanum manganites (La{sub 1−z}Nd{sub z}){sub 1.4}Sr{sub 1.6}Mn{sub 2}O{sub 7} (z = 0 and 0.1) at a transport current flowing along the crystal c axis and in external magnetic fields applied parallel to the crystal c axis or ab plane. It is demonstrated that the La{sub 1.4}Sr{sub 1.6}Mn{sub 2}O{sub 7} manganite exhibits the positive magnetoresistance effect in the magnetic field applied in the ab sample plane at the temperatures T < 60 K, along with the negative magnetoresistance typical of all the substituted lanthanum manganites. In the (La{sub 0.9}Nd{sub 0.1}){sub 1.4}Sr{sub 1.6}Mn{sub 2}O{sub 7} sample, the positive magnetoresistancemore » effect is observed at temperatures of 60–80 K in an applied field parallel to the c axis. The mechanism of this effect is shown to be fundamentally different from the colossal magnetoresistance effect typical of lanthanum manganites. The positive magnetoresistance originates from spin-dependent tunneling of carriers between the manganese-oxygen bilayers and can be explained by features of the magnetic structure of the investigated compounds.« less

Syntheses, structures, and 1H, 13C{ 1H} and 119Sn{ 1H} NMR chemical shifts of a family of trimethyltin alkoxide, amide, halide and cyclopentadienyl compounds

DOE PAGES

Lichtscheidl, Alejandro G.; Janicke, Michael T.; Scott, Brian L.; ...

2015-08-21

The synthesis and full characterization, including Nuclear Magnetic Resonance (NMR) data ( 1H, 13C{ 1H} and 119Sn{ 1H}), for a series of Me 3SnX (X = O-2,6-tBu 2C 6H 3 (1), (Me 3Sn)N(2,6- iPr 2C 6H 3) (3), NH-2,4,6- tBu 3C 6H 2 (4), N(SiMe 3) 2 (5), NEt 2, C 5Me 5 (6), Cl, Br, I, and SnMe 3) compounds in benzene-d 6, toluene-d 8, dichloromethane-d 2, chloroform-d 1, acetonitrile-d 3, and tetrahydrofuran-d 8 are reported. The X-ray crystal structures of Me 3Sn(O-2,6- tBu 2C 6H 3) (1), Me 3Sn(O-2,6- iPr 2C 6H 3) (2), and (Me 3Sn)(NH-2,4,6- tBumore » 3C 6H 2) (4) are also presented. As a result, these compiled data complement existing literature data and ease the characterization of these compounds by routine NMR experiments.« less

A series of Zn/Cd coordination polymers constructed from 1,4-naphthalenedicarboxylate and N-donor ligands: Syntheses, structures and luminescence sensing of Cr{sup 3+} in aqueous solutions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hu, Dong-Cheng; Key Laboratory for Preparation and Application of Ordered Structural Materials of Guangdong Province, Shantou University, Shantou 515063; Fan, Yan

A novel series of Zn/Cd coordination polymers based on H{sub 3}L, namely, [Zn{sub 2}(HL){sub 2}(bipy){sub 2}(H{sub 2}O){sub 6}]{sub n} (1), [Zn(HL)(phen)]{sub n} (2), [Cd{sub 3}L{sub 2}(bbi){sub 3}]{sub n} (3), [Zn{sub 3}L{sub 2}(bbi){sub 3}]{sub n} (4) [(H{sub 3}L =4-[(1-carboxynaphthalen-2-yl)oxy]phthalic acid, bipy =4,4′-bipyridine, phen =1,10-phenanthroline, bbi =1,1′-(1,4-butanediyl)bis(imidazole] have been successfully synthesized by solvothermal reaction. Compound 1 possesses two diverse 1D chains constructed by different bipy coligands, which were further connected to form a 3D supramolecular architecture by hydrogen bonding interactions. Compound 2 possesses a complicated 1D chain based on secondary building unit (SBU) with binuclear Zn cluster. Compounds 3 and 4 exhibitmore » similar 2D→3D framework, which can be rationalized as (3,4,4)-connected 3D net with a Schläfli symbol of (6{sup 3}.8.10{sup 2}){sub 2}(6{sup 3}){sub 2}(6{sup 4}.8.10). In particular, compound 3 exhibited a high sensitivity for Cr{sup 3+} in aqueous solutions, which suggest that compound 3 is a promising luminescent probe for selectively sensing Cr{sup 3+}. - Graphical abstract: A series of novel Zn/Cd coordination polymers have been successfully synthesized by solvothermal reaction. The unique 3D Cd{sup 2+} polymer containing bbi as second ligand demonstrates high sensitivity for detection of toxic Cr{sup 3+} in aqueous solutions. Display Omitted - Highlights: • π-conjugated semirigid tricarboxylate ligands with naphthalene rings(H{sub 3}L) were rationally designed. • Four Zn/Cd coordination polymers based on H{sub 3}L have been successfully synthesized by solvothermal reaction. • Compound 3 is a promising luminescent probe for selectively sensing Cr{sup 3+} with high sensitivity in aqueous solutions.« less

Thermopower of CexR1-xB6 (R=La, Pr and Nd)

NASA Astrophysics Data System (ADS)

Kim, Moo‑Sung; Nakai, Yuki; Tou, Hideki; Sera, Masafumi; Iga, Fumitoshi; Takabatake, Toshiro; Kunii, Satoru

2006-06-01

The thermopower, S, of CexR1-xB6 (R=La, Pr, Nd) was investigated. S with a positive sign shows a typical behavior observed in the Ce Kondo system, an increase with decreasing temperature at high temperatures and a maximum at low temperatures. The S values of all the systems at high temperatures are roughly linearly dependent on the Ce concentration, indicating the conservation of the single-impurity character of the Kondo effect in a wide x range. However, the maximum value of S, Smax, and the temperature, Tmax, at which Smax is observed exhibit different x dependences between CexLa1-xB6 and CexR1-xB6 (R=Pr, Nd). In CexLa1-xB6, Tmax, which is ˜8 K in CeB6, decreases with decreasing x and converges to ˜1 K in a very dilute alloy and Smax shows an increase below x ˜ 0.1 after decreasing with decreasing x. In CexR1-xB6 (R=Pr, Nd), Tmax shows a weak x dependence but Smax shows a roughly linear decrease in x. These results are discussed from the standpoint of the chemical pressure effect and the Ce-Ce interaction. S in the long-range ordered phase shows very different behaviors between CexPr1-xB6 and CexNd1-xB6.

Magnetic ordering in intermetallic La1-xTbxMn2Si2 compounds

NASA Astrophysics Data System (ADS)

Korotin, Dm. M.; Streltsov, S. V.; Gerasimov, E. G.; Mushnikov, N. V.; Zhidkov, I. S.; Kukharenko, A. I.; Finkelstein, L. D.; Cholakh, S. O.; Kurmaev, E. Z.

2018-05-01

The magnetic structures and magnetic phase transitions in intermetallic layered La1-xTbxMn2Si2 compounds (the ThCr2Si2-type structure) are investigated using the first-principles method and XPS measurements. The experimentally observed transition from ferromagnetic (FM) to antiferromagnetic (AFM) ordering of Mn sublattice with increase of terbium concentration is successfully reproduced in calculations for collinear magnetic moments model. The FM →AFM change of interplane magnetic ordering at small x is irrelevant to the number of f-electrons of the rare-earth ion. In contrast it was shown to be related to the Mn-Mn in-plane distance. Calculated Tb critical concentration for this transition x ≈ 0.14 corresponds to the Mn-Mn in-plane distance 0.289 nm, very close to the experimentally observed transition distance 0.287 nm. The crystal cell compression due to substitution increases an overlap between Mndxz,yz and the rare-earth ion d orbitals. Resulting hybridized states manifest themselves as an additional peak in the density of states. We suggest that a corresponding interlayer Mn-R-Mn superexchange interaction stabilizes AFM magnetic ordering in these compounds with Tb doping level x > 0.2 . The results of DFT calculations are in agreement with X-ray photoemission spectra for La1-xTbxMn2Si2 .

Hydrothermal syntheses, crystal structures and luminescence properties of zinc(II) and cadmium(II) coordination polymers based on bifunctional 3,2 Prime :6 Prime ,3 Prime Prime -terpyridine-4 Prime -carboxylic acid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Na; Guo, Hui-Lin; Hu, Huai-Ming, E-mail: ChemHu1@NWU.EDU.CN

2013-02-15

Five new coordination polymers, [Zn{sub 2}(ctpy){sub 2}Cl{sub 2}]{sub n} (1), [Zn{sub 2}(ctpy){sub 2}(ox)(H{sub 2}O){sub 2}]{sub n} (2), [Zn{sub 2}(ctpy)(3-btc)(H{sub 2}O)]{sub n}{center_dot}0.5nH{sub 2}O (3), [Cd(ctpy){sub 2}(H{sub 2}O)]{sub n} (4), [Cd{sub 4}(ctpy){sub 2}(2-btc){sub 2}(H{sub 2}O){sub 2}]{sub n}{center_dot}2nH{sub 2}O (5), (Hctpy=3,2 Prime :6 Prime ,3 Prime Prime -terpyridine-4 Prime -carboxylic acid, H{sub 2}ox=oxalic acid, H{sub 3}(3-btc)=1,3,5-benzenetricarboxylic acid, H{sub 3}(2-btc)=1,2,4-benzenetricarboxylic acid) have been synthesized under hydrothermal conditions and characterized by elemental analysis, IR spectroscopy, and single-crystal X-ray diffraction. Compounds 1-2 are a one-dimensional chain with weak interactions to form 3D supramolecular structures. Compound 3 is a 4-nodal 3D topology framework comprised of binuclear zincmore » units and (ctpy){sup -} anions. Compound 4 shows two dimensional net. Compound 5 is a (4,5,6)-connected framework with {l_brace}4{sup 4}{center_dot}6{sup 2}{r_brace}{l_brace}4{sup 6}{center_dot}6{sup 4}{r_brace}{sub 2}{l_brace}4{sup 9}{center_dot}6{sup 6}{r_brace} topology. In addition, the thermal stabilities and photoluminescence properties of 1-5 were also studied in the solid state. - Graphical abstract: Five new Zn/Cd compounds with 3,2 Prime :6 Prime ,3 Prime Prime -terpyridine-4 Prime -carboxylic acid were prepared. The photoluminescence and thermal stabilities properties of 1-5 were investigated in the solid state. Highlights: Black-Right-Pointing-Pointer Five new zinc/cadmium metal-organic frameworks have been hydrothermal synthesized. Black-Right-Pointing-Pointer The structural variation is attributed to the diverse metal ions and auxiliary ligand. Black-Right-Pointing-Pointer Compounds 1-5 exhibit 1D ring chain, 2D layer and 3D open-framework, respectively. Black-Right-Pointing-Pointer These compounds exhibit strong solid state luminescence emission at room temperature.« less

Syntheses and structural characterization of non-centrosymmetric Na{sub 2}M{sub 2}M'S{sub 6} (M, M′=Ga, In, Si, Ge, Sn, Zn, Cd) sulfides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yohannan, Jinu P.; Vidyasagar, Kanamaluru, E-mail: kvsagar@iitm.ac.in

Seven new non-centrosymmetric Na{sub 2}M{sub 2}M’S{sub 6} sulfides, namely, Na{sub 2}Sn{sub 2}ZnS{sub 6}(1){sub ,} Na{sub 2}Ga{sub 2}GeS{sub 6}(2), Na{sub 2}Ga{sub 2}SnS{sub 6}(3-α), Na{sub 2}Ga{sub 2}SnS{sub 6}(3-β){sub ,} Na{sub 2}Ge{sub 2}ZnS{sub 6}(4){sub ,} Na{sub 2}Ge{sub 2}CdS{sub 6}(5){sub ,} Na{sub 2}In{sub 2}SiS{sub 6}(6) and Na{sub 2}In{sub 2}GeS{sub 6}(7), were synthesized by high temperature solid state reactions and structurally characterized by single crystal X-ray diffraction. They crystallize in non-centrosymmetric Fdd2 and Cc space groups and their three-dimensional [M{sub 2}M′S{sub 6}]{sup 2-}framework structures consist of MS{sub 4} and M′S{sub 4} tetrahedra corner-connected to one another in either orderly or disordered fashion. Sodium ions residemore » in the tunnels of the anionic framework. Compounds 1, 2 and 3-α have the structure of known Li{sub 2}Ga{sub 2}GeS{sub 6}, whereas compounds 6 and 7 are isostructural with known Li{sub 2}In{sub 2}GeS{sub 6} compound. Isostructural compounds 4 and 5 represent a new structural variant. Compounds 3-α and its new monoclinic structural variant 3-β have disordered structural framework. All of them are wide band gap semiconductors. Na{sub 2}Ga{sub 2}GeS{sub 6}(2), Na{sub 2}Ga{sub 2}SnS{sub 6}(3), Na{sub 2}Ge{sub 2}ZnS{sub 6}(4) and Na{sub 2}In{sub 2}GeS{sub 6}(7) compounds are found to be second-harmonic generation (SHG) active. Compounds 1, 2 and 3-α melt congruently. - Graphical abstract: Na{sub 2}Ga{sub 2}GeS{sub 6}, Na{sub 2}Ga{sub 2}SnS{sub 6}, Na{sub 2}Ge{sub 2}ZnS{sub 6}, Na{sub 2}In{sub 2}GeS{sub 6}, Na{sub 2}Sn{sub 2}ZnS{sub 6}, Na{sub 2}Ge{sub 2}CdS{sub 6} and Na{sub 2}In{sub 2}SiS{sub 6} have non-centrosymmetric structures and the first four compounds are SHG active. Display Omitted - Highlights: • Seven new Na{sub 2}M{sub 2}M′S{sub 6} compounds with non-centrosymmetric structures were synthesized. • They are wide band gap semiconductors. • Na{sub 2}Ga{sub 2}GeS{sub 6

Lanthanide contraction effect on crystal structures of lanthanide coordination polymers with cyclohexanocucurbit[6]uril ligand

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zheng, Li-Mei; Liu, Jing-Xin, E-mail: jxliu411@ahut.edu.cn

A series of compounds based on the macrocyclic ligand cyclohexanocucurbit[6]uril (Cy6Q[6]) with formulas (Ln(H{sub 2}O){sub 6}Cy6Q[6])·2(CdCl{sub 4})·H{sub 3}O·xH{sub 2}O [isomorphous with Ln=La (1), Ce (2), Pr (3) and Nd (4), x=11 (1), 11 (2), 10 (3) and 11 (4)], (Sm(H{sub 2}O){sub 5}Cy6Q[6])·2(CdCl{sub 4})·H{sub 3}O·10H{sub 2}O (5) and (Ln(H{sub 2}O){sub 5}(NO{sub 3})@Cy6Q[6])·2(CdCl{sub 4})·2H{sub 3}O·xH{sub 2}O [isomorphous with Ln=Gd (6), Tb (7) and Dy (8), x=8 (6), 6 (7) and 6 (8)], have been successfully synthesized by the self-assembly of Cy6Q[6] with the corresponding lanthanide nitrate under hydrochloric acid aqueous solution in the presence of CdCl{sub 2}. Single-crystal X-ray diffraction analyses revealedmore » that compounds 1–8 all crystallize in monoclinic space group P2{sub 1}/c, and display 1D coordination polymer structures. The lanthanide contraction effect on the structures of 1–8 has also been investigated and discussed in detail. In contrast, the reaction of Cy6Q[6] with the Ho(NO){sub 3}, Tm(NO){sub 3}, Yb(NO){sub 3} under the same conditions resulted in the compounds 9–11 with formulas Cy6Q[6]·2(CdCl{sub 4})·2H{sub 3}O·xH{sub 2}O [isomorphous with x=10 (9), 10 (10), and 9 (11)], in which no lanthanide cations are observed. The structural difference of these compounds indicates that the Cy6Q[6] may be used in the separation of lanthanide cations. - Graphical abstract: The reaction of cyclohexanocucurbit[6]uril with lanthanide ions (La{sup 3+}, Ce{sup 3+}, Pr{sup 3+}, Nd{sup 3+}, Sm{sup 3+}, Gd{sup 3+}, Tb{sup 3+}, Dy{sup 3+}, Ho{sup 3+}, Tm{sup 3+} and Yb{sup 3+}) under hydrochloric acid in the presence of CdCl{sub 2} resulted in eleven compounds, which demonstrate interesting lanthanide contraction effect and provide a means of separating lanthanide ions. - Highlights: • Eleven compounds of the Ln{sup 3+} with the Cy6Q[6] were synthesized and described. • Compounds 1-8 demonstrate interesting lanthanide contraction

Development of (6R)-2-Nitro-6-[4-(trifluoromethoxy)phenoxy]-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazine (DNDI-8219): A New Lead for Visceral Leishmaniasis

PubMed Central

2018-01-01

Discovery of the potent antileishmanial effects of antitubercular 6-nitro-2,3-dihydroimidazo[2,1-b][1,3]oxazoles and 7-substituted 2-nitro-5,6-dihydroimidazo[2,1-b][1,3]oxazines stimulated the examination of further scaffolds (e.g., 2-nitro-5,6,7,8-tetrahydroimidazo[2,1-b][1,3]oxazepines), but the results for these seemed less attractive. Following the screening of a 900-compound pretomanid analogue library, several hits with more suitable potency, solubility, and microsomal stability were identified, and the superior efficacy of newly synthesized 6R enantiomers with phenylpyridine-based side chains was established through head-to-head assessments in a Leishmania donovani mouse model. Two such leads (R-84 and R-89) displayed promising activity in the more stringent Leishmania infantum hamster model but were unexpectedly found to be potent inhibitors of hERG. An extensive structure–activity relationship investigation pinpointed two compounds (R-6 and pyridine R-136) with better solubility and pharmacokinetic properties that also provided excellent oral efficacy in the same hamster model (>97% parasite clearance at 25 mg/kg, twice daily) and exhibited minimal hERG inhibition. Additional profiling earmarked R-6 as the favored backup development candidate. PMID:29461823

The first 3-D LaIII-SrII heterometallic complex: Synthesis, structure and luminescent properties

NASA Astrophysics Data System (ADS)

Hong, Zhiwei; Ran, Jingwen; Li, Tao; Chen, Yanmei

2016-10-01

The first 3-D LaIII-SrII heterometallic complex, namely [La2Sr(pda)4(H2O)4]n·6nH2O (1, H2pda = pyridine-2,6-dicarboxylic acid), has been successfully synthesized under solvothermal conditions. Single crystal X-ray diffraction analysis reveals that complex 1 features a 3-D porous framework and displays a new topology. The crystal structure can be simplified to a 4,6-connected 3-D network with Schläfli symbol of {34·42·88·9}2{34·42}. The crystals also have been characterized by X-ray powder diffraction, elemental analysis, thermal analysis, and IR spectroscopy. The infrared spectral analysis indicates that complex 1 is a carboxylate coordinated compound, several water molecules exist in the compound. The thermal study shows that there are ten water molecules in the crystal structure. The luminescent property has also been investigated. It shows a blue-purple fluorescence emission.

Multiple biological activities and molecular docking studies of newly synthesized 3-(pyridin-4-yl)-1H-pyrazole-5-carboxamide chalcone hybrids.

PubMed

Sribalan, Rajendran; Banuppriya, Govindharasu; Kirubavathi, Maruthan; Jayachitra, A; Padmini, Vediappen

2016-12-01

A series of fifteen new chemical entities, 3-(pyridin-4-yl)-1H-pyrazole-5-carboxamide chalcones (6a-o), were synthesized as new hybrids with enriched biological activities compared to their parent molecules. The compounds were characterized by 1 H NMR, 13 C NMR, Mass and IR spectral studies. Their antibacterial, anti-inflammatory and antioxidant activities have been evaluated. These compounds showed moderate to good antibacterial, anti-inflammatory and antioxidant activities. The molecular docking analysis was performed with cyclooxygenase enzyme to ascertain the probable binding model. Copyright © 2016 Elsevier Ltd. All rights reserved.

New metal-organic frameworks of [M(C6H5O7)(C6H6O7)(C6H7O7)(H2O)] . H2O (M=La, Ce) and [Ce2(C2O4)(C6H6O7)2] . 4H2O

NASA Astrophysics Data System (ADS)

Weng, Sheng-Feng; Wang, Yun-Hsin; Lee, Chi-Shen

2012-04-01

Two novel materials, [M(C6H5O7)(C6H6O7)(C6H7O7)(H2O)] . H2O (M=La(1a), Ce(1b)) and [Ce2(C2O4)(C6H6O7)2] . 4H2O (2), with a metal-organic framework (MOF) were prepared with hydrothermal reactions and characterized with photoluminescence, magnetic susceptibility, thermogravimetric analysis and X-ray powder diffraction in situ. The crystal structures were determined by single-crystal X-ray diffraction. Compound 1 crystallized in triclinic space group P1¯ (No. 2); compound 2 crystallized in monoclinic space group P21/c (No. 14). The structure of 1 is built from a 1D MOF, composed of deprotonated citric ligands of three kinds. Compound 2 contains a 2D MOF structure consisting of citrate and oxalate ligands; the oxalate ligand arose from the decomposition in situ of citric acid in the presence of CuII ions. Photoluminescence spectra of compounds 1b and 2 revealed transitions between the 5d1 excited state and two levels of the 4f1 ground state (2F5/2 and 2F7/2). Compounds 1b and 2 containing CeIII ion exhibit a paramagnetic property with weak antiferromagnetic interactions between the two adjacent magnetic centers.

Property study of poly nitro compounds of cis-syn-cis-2, 6-dioxodecahydro-lH, 5H-diimidazo [4, 5-b: 4', 5'-e] pyrazine

NASA Astrophysics Data System (ADS)

Liu, Yang; Xu, Zhibin; Xu, Yudong; Xu, Liang; Meng, Zihui

2017-03-01

Poly nitro group substituted cis-syn-cis-2, 6-dioxodecahydro-lH, 5H-diimidazo [4, 5-b: 4', 5'-e] pyrazine derivatives are synthesized by modified method and adequately characterized. All compounds have good performance both in density (ρ> 1.85 g/cm3) and high detonation velocity (vD > 8800 m/s, calculated). Some representative compounds, for example, 4 (vD: 9405 ms-1; P: 41.6 GPa) and 5 (vD:9781 ms-1; P: 45.6 GPa) exhibit excellent detonation performances, which are comparable with current energetic compounds such as RDX (vD: 8724 ms-1; P: 35.2 GPa) and HMX (vD:9059 ms-1; P: 39.2 GPa). Considering the sensitivity increasing with the number of nitro group, two componds with tetranitro groups (2 and 3) are worthy of deep research.

Syntheses, Characterization, Resolution, and Biological Studies of Coordination Compounds of Aspartic Acid and Glycine

PubMed Central

Akinkunmi, Ezekiel; Ojo, Isaac; Adebajo, Clement; Isabirye, David

2017-01-01

Enantiomerically enriched coordination compounds of aspartic acid and racemic mixtures of coordination compounds of glycine metal-ligand ratio 1 : 3 were synthesized and characterized using infrared and UV-Vis spectrophotometric techniques and magnetic susceptibility measurements. Five of the complexes were resolved using (+)-cis-dichlorobis(ethylenediamine)cobalt(III) chloride, (+)-bis(glycinato)(1,10-phenanthroline)cobalt(III) chloride, and (+)-tris(1,10-phenanthroline)nickel(II) chloride as resolving agents. The antimicrobial and cytotoxic activities of these complexes were then determined. The results obtained indicated that aspartic acid and glycine coordinated in a bidentate fashion. The enantiomeric purity of the compounds was in the range of 22.10–32.10%, with (+)-cis-dichlorobis(ethylenediamine)cobalt(III) complex as the more efficient resolving agent. The resolved complexes exhibited better activity in some cases compared to the parent complexes for both biological activities. It was therefore inferred that although the increase in the lipophilicity of the complexes may assist in the permeability of the complexes through the cell membrane of the pathogens, the enantiomeric purity of the complexes is also of importance in their activity as antimicrobial and cytotoxic agents. PMID:28293149

Two novel transition metal-organic frameworks based on 1,3,5-benzenetricarboxylate ligand: Syntheses, structures and thermal properties

NASA Astrophysics Data System (ADS)

Fu, Ying; Li, Guobao; Liao, Fuhui; Xiong, Ming; Lin, Jianhua

2011-10-01

Two novel transition metal-organic frameworks, [Zn 6(OH) 3(BTC) 3(H 2O) 3]ṡ7H 2O ( 1) and [Cd(BTC)(H 2O)]ṡ[HIM] ( 2) (H 3BTC = 1,3,5-benzenetricarboxylic acid), have been synthesized under hydrothermal conditions and characterized by single crystal and variable temperature powder X-ray diffraction (VTPXRD), IR spectroscopy, elemental analyses, ICP measurements, and coupled TG-MS analyses. Compound 1 crystallizes in the trigonal space group R3 c, and could be described as a 3D porous network consisting of (Zn 2O 8) n zigzag chains and bridging BTC ligands with 1D channels along c axis. Compound 2 crystallizes in the monoclinic space group P2 1/ c, and exhibits a 2D framework made up of CdO 6 octahedra and BTC ligands parallel the bc plane. TG-MS and VTPXRD studies reveal that 1 is stable up to 320 °C under air, and 2 stable up to 220 °C.

Synthesis of 4-((1E, 6E)-7-(4-hydroxy-3-methoxyphenyl)-3, 5-dioxohepta-1, 6-dienyl)-2-methoxyphenyl 4-fluorobenzoate, a novel monoester derivative of curcumin, its experimental and theoretical (DFT) studies

NASA Astrophysics Data System (ADS)

Srivastava, Sangeeta; Gupta, Preeti; Amandeep; Singh, Ranvijay Pratap

2016-04-01

Curcumin (1), isolated as a major component from the chloroform extract of Curcuma longa was converted to its ester derivative 4-((1E, 6E)-7-(4-hydroxy-3-methoxyphenyl)-3,5-dioxohepta-1,6-dienyl)-2-methoxyphenyl 4-fluorobenzoate (2). The compound has been characterized with the help of 1H, 13C NMR, UV, IR and mass spectrometry. The molecular geometry of synthesized compound was calculated in ground state by Density functional theory (DFT/B3LYP) using 6-31G (d,p) basis set. 1H and 13C NMR chemical shifts were calculated in ground state by using Gauge-Including Atomic Orbital (GIAO) approach and these values were correlated with experimental observations. The electronic properties such as HOMO and LUMO energies were calculated using time dependent Density Functional Theory (TD-DFT). Stability of the molecule as a result of hyper conjugative interactions and electron delocalization were analysed using Natural bond orbital (NBO) analysis. Intramolecular interactions were analysed by AIM (Atom in molecule) approach. Global reactivity descriptors were calculated to study the reactive site within molecule. The vibrational wavenumbers were calculated using DFT method and assigned with the help of potential energy distribution (PED). First hyperpolarizability values have been calculated to describe the nonlinear optical (NLO) property of the synthesized compounds. Molecular electrostatic potential (MEP) analysis has also been carried out.

SYNTHESIS AND BIOLOGICAL EVALUATION OF N-(SUBSTITUTED PHENYL)-2-(5H-[1,2,4]TRIAZINO[5,6-b]INDOL-3-YLSULFANYL)ACETAMIDES AS ANTIMICROBIAL, ANTIDEPRESSANT AND ANTICONVULSANT AGENTS.

PubMed

Shruthi, N; Poojary, Boja; Kumar, Vasantha; Prathibha, A; Hussain, Mumtaz Mohammed; Revanasiddappa, B C; Joshi, Himanshu

2015-01-01

A new series of N-Aryl-2-(5H-[1,2,4]triazino[5,6-b]indol-3-ylsulfanyl)acetamides were synthesized by condensation of tricyclic compound 2,5-dihydro-3H-[1,2,4]triazino[5,6-b]indole-3-thione with chloro N-phenylacetamides. The tricyclic compound was obtained by condensation of Isatin with thiosemicarbazide. Chloro N-phenylacetamides were obtained from different substituted anilines. Their structures were characterized by IR, 1H NMR, LC-MS and elemental analyses. Newly synthesized compounds were screened for antimicrobial, antidepressant and anticonvulsant activities. Preliminary results indicated that most of the compounds showed lesser MIC value than the standard drug used when tested for antimicrobial activity. Some of the compounds were endowed with very good antidepressant and anticonvulsant activity.

Rare ginsenoside Ia synthesized from F1 by cloning and overexpression of the UDP-glycosyltransferase gene from Bacillus subtilis: synthesis, characterization, and in vitro melanogenesis inhibition activity in BL6B16 cells.

PubMed

Wang, Dan-Dan; Jin, Yan; Wang, Chao; Kim, Yeon-Ju; Perez, Zuly Elizabeth Jimenez; Baek, Nam In; Mathiyalagan, Ramya; Markus, Josua; Yang, Deok-Chun

2018-01-01

Ginsenoside F1 has been described to possess skin-whitening effects on humans. We aimed to synthesize a new ginsenoside derivative from F1 and investigate its cytotoxicity and melanogenesis inhibitory activity in B16BL6 cells using recombinant glycosyltransferase enzyme. Glycosylation has the advantage of synthesizing rare chemical compounds from common compounds with great ease. UDP-glycosyltransferase (BSGT1) gene from Bacillus subtilis was selected for cloning. The recombinant glycosyltransferase enzyme was purified, characterized, and utilized to enzymatically transform F1 into its derivative. The new product was characterized by NMR techniques and evaluated by MTT, melanin count, and tyrosinase inhibition assay. The new derivative was identified as (20 S )-3 β ,6 α ,12 β ,20-tetrahydroxydammar-24-ene-20- O - β -D-glucopyranosyl-3- O - β -D-glucopyranoside (ginsenoside Ia), which possesses an additional glucose linked into the C-3 position of substrate F1. Ia had been previously reported; however, no in vitro biological activity was further examined. This study focused on the mass production of arduous ginsenoside Ia from accessible F1 and its inhibitory effect of melanogenesis in B16BL6 cells. Ia showed greater inhibition of melanin and tyrosinase at 100 μmol/L than F1 and arbutin. These results suggested that Ia decreased cellular melanin synthesis in B16BL6 cells through downregulation of tyrosinase activity. To our knowledge, this is the first study to report on the mass production of rare ginsenoside Ia from F1 using recombinant UDP-glycosyltransferase isolated from B. subtillis and its superior melanogenesis inhibitory activity in B16BL6 cells as compared to its precursor. In brief, ginsenoside Ia can be applied for further study in cosmetics.

Photoresponse and DFT studies of new synthesized 2-benzylidene-3-hydroxy -1-(5,6-diphenyl-1,2,4-triazine-3-yl)hydrazine and optical sensor application

NASA Astrophysics Data System (ADS)

Taha, A.; Farag, A. A. M.; Adly, O. M. I.; Roushdy, N.; Shebl, Magdy; Ahmed, H. M.

2017-08-01

A newly Schiff base,2-benzylidene-3-hydroxy-1-(5,6-diphenyl-1,2,4-triazine-3-yl)hydrazine] (HBDHT) was synthesized and characterized on the basis of micro-analytical and spectroscopic studies. Basic parameters of the combined compound HBDHT were ascertained on the premise of DFT level actualized on Gaussian 09. Thin films of HBDHT were successfully prepared by spin coating technique and confirmed by atomic force microscopy (AFM). The optical attributes of the studied films were considered utilizing spectrophotometric estimations in a wide spectral range of 200-2500 nm. Some important optical parameters such as extinction index, refractive index, dispersion energy, oscillator energy and high-frequency dielectric constant were extracted. Analysis of the absorption coefficient near the fundamental absorption edge confirms an indirectly allowed transition with an energy gap of 1.7eV. The refractive index dispersion was estimated on basis of single oscillator model expressed by Wemple-Didomenico. Current-voltage (I-V) characteristics were studied in dark and under illumination of 100 mW/cm2 to clarify the sensitivity to light. Moreover, the photo-transient properties were also investigated to confirm that the prepared heterojunction based HBDHT can be operated as a photodiode.

ADP-ribosyl-N₃: A Versatile Precursor for Divergent Syntheses of ADP-ribosylated Compounds.

PubMed

Li, Lingjun; Li, Qianqian; Ding, Shengqiang; Xin, Pengyang; Zhang, Yuqin; Huang, Shenlong; Zhang, Guisheng

2017-08-14

Adenosine diphosphate-ribose (ADP-ribose) and its derivatives play important roles in a series of complex physiological procedures. The design and synthesis of artificial ADP-ribosylated compounds is an efficient way to develop valuable chemical biology tools and discover new drug candidates. However, the synthesis of ADP-ribosylated compounds is currently difficult due to structural complexity, easily broken pyrophosphate bond and high hydrophilicity. In this paper, ADP-ribosyl-N₃ was designed and synthesized for the first time. With ADP-ribosyl-N₃ as the key precursor, a divergent post-modification strategy was developed to prepare structurally diverse ADP-ribosylated compounds including novel nucleotides and peptides bearing ADP-ribosyl moieties.

Diastereoselective syntheses of 3-aryl-5-(arylalkyl)-6-methyl-1-(1-phenylethyl)thioxotetrahydropyrimidin-4(1H)-ones: a stereochemical perspective from endo and exocyclic chiral centres.

PubMed

Kumar, Varun; Raghavaiah, Pallepogu; Mobin, Shaikh M; Nair, Vipin A

2010-11-07

Diastereoselective syntheses of 3-aryl-(S/R)-6-methyl-1-[(S/R)-1-phenylethyl)]-2-thioxotetrahydro pyrimidin-4(1H)-ones were achieved in good yields by the condensation of aryl isothiocyanates with ethyl 3-(1-phenylethylamino)butanoate in a one-pot reaction. Benzylation of these substrates illustrated that the orientations of the exocylic and endocylic groups determine the stereochemical outcome of the product formed.

Mass spectral analysis of long chain alkyl aromatic compounds synthesized from alpha-olefin alkylation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cheng, M.T.; Hudson, J.D.

1994-12-31

Long chain alkyl aromatic compounds are important petrochemicals with many applications. They are generally synthesized by alkylating the corresponding aromatic nucleus. In this report, the authors will describe the mass spectral fragmentation of alkylphenols and alkylsalicylates.

Structural, magnetic, magneto-caloric and Mössbauer spectral study of Tb{sub 2}Fe{sub 17} compound synthesized by arc melting

DOE Office of Scientific and Technical Information (OSTI.GOV)

Charfeddine, S.; LVMU, Centre National de Recherches en Sciences des Matériaux, Technopole de Borj-Cédria, BP 73 Soliman 8027; Zehani, K.

We have synthesized the intermetallic Tb{sub 2}Fe{sub 17} compound in hexagonal crystal structure by arc-melting without annealing. X-ray diffraction pattern has been refined by Rietveld method. The crystal structure is hexagonal with P6{sub 3}/mmc space group (Th{sub 2}Ni{sub 17}-type). The Mössbauer spectrum of Tb{sub 2}Fe{sub 17} compound has been analyzed with seven magnetic sextets assigned to the inequivalent crystallographic sites. The temperature dependence of magnetization data revealed that Tb{sub 2}Fe{sub 17} exhibits a second-order ferromagnetic to paramagnetic phase transition in the vicinity of Curie temperature (T{sub C}=412 K). The relative cooling power around the magnetic transition and the Arrott plotsmore » are also reported. - Graphical abstract: A 3D surface showing the temperature and applied magnetic field dependencies of the magnetization for Tb{sub 2}Fe{sub 17} compound (left). Rietveld analysis of the XRD pattern (right). Crystal structure for the hexagonal P6{sub 3}/mmc Tb{sub 2}Fe{sub 17} (bottom). Display Omitted - Highlights: • Tb{sub 2}Fe{sub 17} single-phase synthesized by simple arc-melting without any heat treatment. • The crystal structure is hexagonal with P6{sub 3}/mmc space group. • The magnetic entropy change of the sample was determined by Maxwell relation. • Hyperfine parameters, magnetic and magnetocaloric properties were studied.« less

Design and synthesis of positional isomers of 5 and 6-bromo-1-[(phenyl)sulfonyl]-2-[(4-nitrophenoxy)methyl]-1H-benzimidazoles as possible antimicrobial and antitubercular agents.

PubMed

Ranjith, P Karuvalam; Rajeesh, P; Haridas, Karickal R; Susanta, Nayak K; Row, Tayur N Guru; Rishikesan, R; Kumari, N Suchetha

2013-09-15

In this Letter, we report the structure-activity relationship (SAR) studies on series of positional isomers of 5(6)-bromo-1-[(phenyl)sulfonyl]-2-[(4-nitrophenoxy)methyl]-1H-benzimidazoles derivatives 7(a-j) and 8(a-j) synthesized in good yields and characterized by (1)H NMR, (13)C NMR and mass spectral analyses. The crystal structure of 7a was evidenced by X-ray diffraction study. The newly synthesized compounds were evaluated for their in vitro antibacterial activity against Staphylococcus aureus, (Gram-positive), Escherichia coli and Klebsiella pneumoniae (Gram-negative), antifungal activity against Candida albicans, Aspergillus flavus and Rhizopus sp. and antitubercular activity against Mycobacterium tuberculosis H37Rv, Mycobacterium smegmatis, Mycobacterium fortuitum and MDR-TB strains. The synthesized compounds displayed interesting antimicrobial activity. The compounds 7b, 7e and 7h displayed significant activity against Mycobacterium tuberculosis H37Rv strain. Copyright © 2013 Elsevier Ltd. All rights reserved.

Syntheses, structure and magnetic properties of two vanadate garnets Ca{sub 5}M{sub 4}V{sub 6}O{sub 24} (M=Co, Ni)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Nannan; College of Materials Science and Engineering, Fuzhou University, Fuzhou, Fujian 350108; He, Zhangzhen, E-mail: hcz1988@hotmail.com

2015-08-15

Two vanadate compounds Ca{sub 5}M{sub 4}V{sub 6}O{sub 24} (M=Co, Ni) have been synthesized by a high-temperature solid-state reaction. The compounds are found to crystallize in the cubic system with a space group Ia-3d, which exhibit a typical garnet structural framework. Magnetic measurements show that Ca{sub 5}M{sub 4}V{sub 6}O{sub 24} (M=Co, Ni) exhibit similar magnetic behaviors, in which Ca{sub 5}Co{sub 4}V{sub 6}O{sub 24} possesses an antiferromagnetic ordering at T{sub N}=~6 K while Ca{sub 5}Ni{sub 4}V{sub 6}O{sub 24} shows an antiferromagnetic ordering at T{sub N}=~7 K. - Graphical abstract: Garnet vanadate compounds Ca{sub 5}M{sub 4}V{sub 6}O{sub 24} (M=Co, Ni) have been synthesizedmore » by a high-temperature solid-state reaction. Structural features and magnetic behaviors are also investigated. - Highlights: • New type of garnet vanadates Ca{sub 5}M{sub 4}V{sub 6}O{sub 24} (M=Co, Ni) are synthesized by a high-temperature solid-state reaction. • Structural features are confirmed by single crystal samples. • Magnetic behaviors are firstly investigated in the systems.« less

Supramolecular architectures constructed by lanthanum, amino acids and 1,10-phenanthroline via non-covalent bond interactions

NASA Astrophysics Data System (ADS)

Zheng, Xiang-Jun; Jin, Lin-Pei

2003-07-01

Three supramolecular lanthanum coordination compounds of amino acids, with 1,10-phenanthroline (phen), [La 2(APA) 6(phen) 2(H 2O) 2](ClO 4) 6(phen) 4·2H 2O ( 1), [La 2(ABA) 6(phen) 2(H 2O) 2](ClO 4) 6 (phen) 6·4H 2O ( 2), and [La 2(AHA) 4(phen) 4](ClO 4) 6(phen) 4·2H 2O ( 3) (APA=3-aminopropionic acid; ABA=4-aminobutanoic acid; AHA=6-aminohexanoic acid) were synthesized and characterized by single crystal X-ray diffraction. The results show that the three coordination compounds are all composed of binuclear coordination cations built by metal-ligand coordination. Through hydrogen bonding and π-π stacking interactions, complex 1 forms a two-dimensional supramolecular sheet structure extending in the (001) plane, complex 2 forms a three-dimensional supramolecular network with many cavities occupied by ClO 4- and lattice H 2O molecules, and complex 3 forms a two-dimensional supramolecular lamellar structure in the (100) plane.

1E7-03, a low MW compound targeting host protein phosphatase-1, inhibits HIV-1 transcription

PubMed Central

Ammosova, Tatyana; Platonov, Maxim; Ivanov, Andrei; Kont, Yasemin Saygideğer; Kumari, Namita; Kehn-Hall, Kylene; Jerebtsova, Marina; Kulkarni, Amol A; Üren, Aykut; Kovalskyy, Dmytro; Nekhai, Sergei

2014-01-01

Background and Purpose HIV-1 transcription is activated by the Tat protein which recruits the cyclin-dependent kinase CDK9/cyclin T1 to TAR RNA. Tat binds to protein phosphatase-1 (PP1) through the Q35VCF38 sequence and translocates PP1 to the nucleus. PP1 dephosphorylates CDK9 and activates HIV-1 transcription. We have synthesized a low MW compound 1H4, that targets PP1 and prevents HIV-1 Tat interaction with PP1 and inhibits HIV-1 gene transcription. Here, we report our further work with the 1H4-derived compounds and analysis of their mechanism of action. Experimental Approach Using the 1H4-PP1 complex as a model, we iteratively designed and synthesized follow-up libraries that were analysed for the inhibition of HIV-1 transcription and toxicity. We also confirmed the mechanism of action of the PP1-targeting molecules by determining the affinity of binding of these molecules to PP1, by analysing their effects on PP1 activity, disruption of PP1 binding to Tat and shuttling of PP1 to the nucleus. Key Results We identified a tetrahydroquinoline derivative, compound 7, which disrupted the interaction of Tat with PP1. We further optimized compound 7 and obtained compound 7c, renamed 1E7-03, which inhibited HIV-1 with low IC50 (fivefold lower than the previously reported compound, 1H4), showed no cytotoxicity and displayed a plasma half-life greater than 8 h in mice. 1E7-03 bound to PP1 in vitro and prevented shuttling of PP1 into the nucleus. Conclusions and Implications Our study shows that low MW compounds that functionally mimic the PP1-binding RVxF peptide can inhibit HIV-1 transcription by deregulating PP1. PMID:25073485

The effects of different heat treatment annealing on structural properties of LaFe11.5Si1.5 compound

NASA Astrophysics Data System (ADS)

Norizan, Yang Nurhidayah Asnida; Din, Muhammad Faiz Md; Zamri, Wan Fathul Hakim W.; Hashim, Fakroul Ridzuan; Jusoh, Mohd Taufik; Rahman, Mohd Rashid Abdul

2018-02-01

The cubic NaZn13-type LaFe13-xSix based compounds have been studied systematically and has become one of the most interesting systems for exploring large MCE. Its magnetic properties are strongly doping dependent and provides many of advantage compare to other as magnetic materials for magnetic refrigerator application. In other to produce high quality of cubic NaZn13-type structure, the structural properties of LaFe11.5Si1.5 compounds annealed at different temperature have been investigated. The LaFe11.5Si1.5 compounds was prepared by arc melting and annealed at two different heat treatment which are 1323 K for 14 days and 1523 K for 4 hour. The powder X-ray diffraction (XRD) shows that a short time and high temperature annealing process has benefits for the formation of the NaZn13-type phase compared to a long time and low temperature annealing process. This is shown by the weight fraction of cubic NaZn13- type structure increases from 80% for low temperature annealing to 83% for high temperature annealing. At the same time, high temperature annealing increase the main structure and decrease the impurity (α-Fe and LaFeSi). Furthermore, it can be clearly seen in the Rietveld refinement results that the lattice parameter is increase at the high temperature annealing because of more cubic NaZn13 is formed at higher temperature.

Design, synthesis and evaluation of dialkyl 4-(benzo[d][1,3]dioxol-6-yl)-1,4-dihydro-2,6-dimethyl-1-substituted pyridine-3,5-dicarboxylates as potential anticonvulsants and their molecular properties prediction.

PubMed

Prasanthi, G; Prasad, K V S R G; Bharathi, K

2013-08-01

The present study is on the development of dialkyl 4-(benzo[d][1,3]dioxol-6-yl)-1,4-dihydro-2,6-dimethyl-1-substituted pyridine-3,5-dicarboxylate derivatives as isosteric analogues of isradipine and nifedipine, by the replacement of benzofurazanyl and 2-nitrophenyl groups respectively with benzo[d][1,3]dioxo-6-yl group, as potential anticonvulsants. Fivfteen new derivatives (8a-8o) were synthesized and tested for anticonvulsant activity using maximal electroshock and subcutaneous pentylenetetrazole induced seizure methods. Compound 8f possessing free NH group in 1,4-dihydropyridine ring, diethyl ester functionality at the positions 3 and 5 showed significant anticonvulsant and antioxidant activities. This was also supported by molecular properties prediction data. Selected compounds were evaluated for antinociceptive activity in capsaicin induced nociception assay at 10 mg/kg body weight, but displayed no significant activity at the tested dose. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

Influence of La/W ratio on electrical conductivity of lanthanum tungstate with high La/W ratio

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kojo, Gen; Shono, Yohei; Ushiyama, Hiroshi

The proton-conducting properties of lanthanum tungstates (LWOs) with high La/W ratios were investigated using electrochemical measurements and quantum chemical calculations. Single phases of LWOs with high La/W ratios (6.3≤La/W≤6.7) were synthesized by high-temperature sintering at around 1700 °C. The electrical conductivity of LWO increased with increasing La/W ratio in the single-phase region. The LWO synthesized at the optimum sintering temperature and time, and with the optimum La/W ratio gave the maximum conductivity, i.e., 2.7×10{sup −3} S cm{sup −1} with La/W=6.7 at 500 °C. Density functional theory calculations, using the nudged elastic band method, were performed to investigate the proton diffusionmore » barrier. The results suggest that the proton diffusion paths around La sites have the lowest proton diffusion barrier. These findings improve our understanding of LWO synthesis and the proton-conducting mechanism and provide a strategy for improving proton conduction in LWOs. - Graphical abstract: The LWOs with high La/W ratios were synthesized for the first time. The optimum La/W ratio gave the maximum conductivity with La/W=6.7 at 500 °C. The proton diffusion paths were also considered with density functional theory calculations. - Highlights: • The proton-conducting properties of lanthanum tungstates (LWOs) were investigated. • Single phase LWOs with high La/W ratios (6.3≤La/W≤6.7) were synthesized successfully. • LWOs with the high La/W ratios showed high proton conductivity. • The DFT calculation suggested the lowest proton diffusion barrier in the path around La sites.« less

Synthesis and crystal structures of new oxyapatites BiCa{sub 4-x}La{sub x}(VO{sub 4}){sub 3-x}(GeO{sub 4}){sub x}O, x=1-3

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhuravlev, V.D., E-mail: zhvd@ihim.uran.ru; Tyutyunnik, A.P.; Zubkov, V.G.

2012-10-15

New germanate-vanadates with the general formula BiCa{sub 4-x}La{sub x}(VO{sub 4}){sub 3-x}(GeO{sub 4}){sub x}O, x=1-3, have been synthesized by the nitrate-citrate method and characterized. Structural refinement based on X-ray powder diffraction data showed that these compounds are isostructural with BiCa{sub 4}(VO{sub 4}){sub 3}O (space group P6{sub 3}/m (N 176), Z=2, a=9.8327-9.8755(3), and c=7.1203-7.2133(2) ). They may be viewed as continuous series of solid solutions where Ca{sup 2+} and V{sup 5+} cations in the crystal lattice of vanadate BiCa{sub 4}(VO{sub 4}){sub 3}O are replaced by La{sup 3+} and Ge{sup 4+} cations. In the process of substitution, the La{sup 3+} cations occupy mainlymore » the 4f lattice sites of the germanate-vanadate oxyapatites, but the filling of the 4f and 6h lattice sites in the germanate BiCaLa{sub 3}(GeO{sub 4}){sub 3} is equivalent. IR and Raman spectra were studied. The Raman spectra clearly show a two-mode behavior: the lines of GeO{sub 4} and VO{sub 4} are separated from each other, and the (V/Ge)O{sub 4} tetrahedra exhibit a quasi-independent behavior. - Graphical abstract: Schematic drawing of the BiCa{sub 3}La(VO{sub 4}){sub 2}(GeO{sub 4})O structure in projection on the ac plane. Green-V and Ge, red-Ca(1) and La(1), yellow-Ca(2), La(2) and Bi, dark-blue-O(1)-O(4), blue-O(5). Highlights: Black-Right-Pointing-Pointer The citrate synthesis of germanate-vanadate oxyapatites. Black-Right-Pointing-Pointer The synthesized compounds crystallize in the hexagonal symmetry. Black-Right-Pointing-Pointer A single series of solid solutions BiCa{sub 4-x}La{sub x}(VO{sub 4}){sub 3-x}(GeO{sub 4}){sub x}O, (x=0-3). Black-Right-Pointing-Pointer IR an Raman spectra of mixed crystals.« less

Spectroscopic studies and structure of 3-methoxy-2 -[(2,4,4,6,6-pentachloro-1,3,5,2{lambda}{sup 5},4{lambda}{sup 5},6{lambda}{sup 5}-triazatriphosphin-2-yl)oxy] benzaldehyde

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oezay, H.; Yildiz, M., E-mail: myildiz@comu.edu.tr; Uenver, H.

2013-01-15

The compound called 3-methoxy-2- [(2,4,4,6,6-pentachloro-1,3,5,2{lambda}{sup 5},4{lambda}{sup 5},6{lambda}{sup 5}-triazatriphosphin-2-yl)oxy] benzaldehyde has been synthesized from the reaction of 2-hydroxy-3-methoxybenzaldehyde with hexachlorocyclotriphosphazene. It has been characterized by elemental analysis, MS, IR, {sup 1}H NMR, {sup 13}C NMR, {sup 31}P NMR and UV-visible spectroscopic techniques. The structure of the title compound has been determind by X-ray analysis. Crystals are orthorhombic, space group P2{sub 1}2{sub 1}2{sub 1}, Z = 4, a = 7.705(1), b = 12.624(1), c = 17.825(2) A, R{sub 1} = 0.0390 and wR{sub 2} = 0.1074 [I > 2{sigma}(I)], respectively.

Synthesis, Antitumor Activity, and Mechanism of Action of 6-Acrylic Phenethyl Ester-2-pyranone Derivatives

PubMed Central

Fang, Sai; Chen, Lei; Yu, Miao; Cheng, Bao; Lin, Yongsheng; Morris-Natschke, Susan L.; Lee, Kuo-Hsiung; Gu, Qiong; Xu, Jun

2015-01-01

Based on the scaffolds of caffeic acid phenethyl ester (CAPE) as well as bioactive lactone-containing compounds, 6-acrylic phenethyl ester-2-pyranone derivatives were synthesized and evaluated against five tumor cell lines (HeLa, C6, MCF-7, A549, and HSC-2). Most of the new derivatives exhibited moderate to potent cytotoxic activity. Moreover, HeLa cell lines showed higher sensitivity to these compounds. Particularly, compound 5o showed potent cytotoxic activity (IC50 = 0.50 – 3.45 μM) against the five cell lines. Further investigation on the mechanism of action showed that 5o induced apoptosis, arrested the cell cycle at G2/M phases in HeLa cells, and inhibited migration through disruption of the actin cytoskeleton. In addition, ADME properties were also calculated in silico, and compound 5o showed good ADMET properties with good absorption, low hepatotoxicity, and good solubility, and thus, could easily be bound to carrier proteins, without inhibition of CYP2D6. A structure-activity relationship (SAR) analysis indicated that compounds with ortho-substitution on the benzene ring exhibited obviously increased cytotoxic potency. This study indicated that compound 5o is a promising compound as an antitumor agent. PMID:25800703

Synthesis, spectroscopic characterization, theoretical study and anti-hepatic cancer activity study of 4-(1E,3Z,6E)-3-hydroxy-7-(4-hydroxy-3-methoxyphenyl)-5-oxohepta-1,3,6-trien-1-yl)-2-methoxyphenyl 4-nitrobenzoate, a novel curcumin congener

NASA Astrophysics Data System (ADS)

Srivastava, Sangeeta; Gupta, Preeti; Singh, Ranvijay Pratap; Jafri, Asif; Arshad, M.; Banerjee, Monisha

2017-08-01

In the present work 4-(1E,3Z,6E)-3-hydroxy-7-(4-hydroxy-3-methoxyphenyl)-5-oxohepta-1,3,6-trien-1-yl)-2-methoxyphenyl 4-nitrobenzoate (2), a novel curcumin ester was synthesized. The molecular structure and spectroscopic analysis were performed using experimental techniques like FT-IR, 1H,13C NMR, mass and UV-visible as well as theoretical calculations. The theoretical calculations were done by DFT level of theory using B3LYP/6-31G (d,p) basis set. The vibrational wavenumbers were calculated using DFT method and assigned with the help of potential energy distribution (PED). The electronic properties such as frontier orbitals and band gap energies have been calculated using time dependent density functional theory (TD-DFT). The strength and nature of weak intramolecular interactions have been studied by AIM approach. Global and local reactivity descriptors have been computed to predict reactivity and reactive sites in the molecule. First hyperpolarizability values have been calculated to describe the nonlinear optical (NLO) property of the synthesized compounds. Molecular electrostatic potential (MEP) analysis has also been carried out. The anti-hepatic cancer activity of compound 2 was also carried out.

Characterization of La2Mo2O9 aerogels synthesized by the sol-gel chemistry and high-temperature supercritical drying.

PubMed

Kersen, Ulo; Keiski, Riitta

2005-10-01

A lanthanum molybdate aerogel, La2Mo2O9, with a mean particle size in the range from 100 to 150 nm, was synthesized by the sol-gel method and high-temperature supercritical drying. In this communication it is shown that control over the crystallinity of product aerogels can be exercised by changing the amount of water used for hydrolysis and the temperature for subsequent heat treatment. Methoxy species are formed on the surface during synthesis. The new aerogel may prove useful as a catalyst for the oxidation of hydrocarbons to oxygenated organic compounds.

Appearance of the octupole ordered phase IV in CexLa1 -x B6

NASA Astrophysics Data System (ADS)

Sera, M.; Kunimori, K.; Matsumura, T.; Kondo, A.; Tanida, H.; Tou, H.; Iga, F.

2018-05-01

We investigated the physical properties of CexLa1 -xB6 at x ˜0.8 , below which the Tβ-type antiferro-octupole (AFO) ordered phase IV appears as a result of the larger suppression rate of TQ than TN by La doping. The most important result is that while the peak of the specific heat at TQ is rapidly suppressed and broadened by La doping, that at TIV is sharp and large. This indicates that although the Tβ-AFO order in the phase IV is robust against the local lattice distortion induced by La doping, the Ox y-type antiferroquadrupole (AFQ) ordered phase II is very weak. The Tx y z-AFO interaction is robust against La doping from the observation of the pronounced enhancement of TQ even in a small x region. Based on these La-doping effect of the multipole interactions, we carried out the mean-field calculation for the four-sublattice model to reproduce the magnetic phase diagrams of CexLa1 -xB6 . Based on the calculated results, we propose that the small splitting of the quartet is induced by La doping in phase I to explain the magnetic phase diagram for x <0.65 . We could obtain the calculated results roughly consistent with the experimental results, although there appear new problems. We classified the mechanisms of the four different types of the competition among the four interactions with roughly the same magnitude, which induce the interesting and complicated properties in CexLa1 -xB6 .

Synthesis, Spatial Structure and Analgesic Activity of Sodium 3-Benzylaminocarbonyl-1-methyl-2,2-dioxo-1H-2λ6,1-benzothiazin-4-olate Solvates

PubMed Central

Ukrainets, Igor V.; Petrushova, Lidiya A.; Shishkina, Svitlana V.; Grinevich, Lina A.; Sim, Galina

2016-01-01

In order to obtain and then test pharmocologically any possible conformers of the new feasible analgesic N-benzyl-4-hydroxy-1-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxamide, its 4-O-sodium salt was synthesized using two methods. X-ray diffraction study made possible to determine that, depending on the chosen synthesis conditions, the above-mentioned compound forms either monosolvate with methanol or monohydrate, where organic anion exists in the form of three different conformers. Pharmacological testing of the two known pseudo-enantiomeric forms of the original N-benzylamide and of the two solvates of its sodium salt was performed simultaneously under the same conditions and in equimolar doses. Comparison of the results obtained while studying the peculiarities of the synthesized compounds spatial structure and biological properties revealed an important structure-action relationship. In particular, it was shown that the intensity of analgesic effect of different conformational isomers of N-benzyl-4-hydroxy-1-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxamide may change considerably: while low active conformers are comparable with piroxicam, highly active conformers are more than twice as effective as meloxicam. PMID:27775559

Influence of interstitial V on structure and properties of ferecrystalline ([SnSe]{sub 1.15}){sub 1}(V{sub 1+x}Se{sub 2})n for n=1, 2, 3, 4, 5, and 6

DOE Office of Scientific and Technical Information (OSTI.GOV)

Falmbigl, M.; Putzky, D.; Ditto, J.

2015-11-15

A series of ferecrystalline compounds ([SnSe]{sub 1.15}){sub 1}(V{sub 1+x}Se{sub 2}){sub n} with n=1–6 and a thin film V{sub 1+x}Se{sub 2} were synthesized utilizing the modulated elemental reactant technique. The effect of interstitial V-atoms ranging from 0.13≤x≤0.42 in different compounds on structure and electrical properties of these intergrowth compounds is reported. The presence of the interstitial V-atoms for n>1 was confirmed by Rietveld refinements as well as HAADF-STEM cross sections. The off-stoichiometry in the thin film V{sub 1.13}Se{sub 2} causes a suppression of the charge density wave, similar to the effect of non-stoichiometry observed for the bulk compound. The charge densitymore » wave of ([SnSe]{sub 1.15}){sub 1}(V{sub 1+x}Se{sub 2}){sub 1,} however, is not affected by the non-stoichiometry due to its incorporation as volume inclusions or due to the quasi 2-dimensionality of the isolated VSe{sub 2} layer. In the compounds ([SnSe]{sub 1.15}){sub 1}(V{sub 1+x}Se{sub 2}){sub n} with n=2–6, the temperature dependence of the electrical resistivity approaches bulk-like behavior. - Highlights: • Ferecrystalline thin film compounds with interstitial V-atoms were synthesized. • Interstitial atoms cause an expansion of the superlattice. • The charge density wave transition in the V{sub 1.13}VSe{sub 2} film is strongly suppressed. • Interstitial V has a minor influence on the CDW transition of the ferecrystals.« less

One-pot three-component Biginelli-type reaction to synthesize 3,4-dihydropyrimidine-2-(1H)-ones catalyzed by Co phthalocyanines: Synthesis, characterization, aggregation behavior and antibacterial activity.

PubMed

Medyouni, Rawdha; Elgabsi, Wissal; Naouali, Olfa; Romerosa, Antonio; Sulaiman Al-Ayed, Abdullah; Baklouti, Lasaad; Hamdi, Naceur

2016-10-05

The synthesis of a novel phthalonitrile derivative with pyridine-2-thiol and 2,4,6-trimethylphenylamine substituents functionalized groups and its peripherally tetrasubstituted cobalt phthalocyanine and cationic phthalocyanines complexes were reported. The aggregation investigations carried out in different concentrations indicate that Co Phthalocyanines compounds 3,4 do not have any aggregation behavior for the concentration range of 6×10(-4)-14×10(-6)M in DMSO. The ion binding properties of Co Phthalocyanines compounds 3,4 show the formation of stable complex with Co(2+). In addition 3,4-Dihydropyrimidin-2(1H)-one derivatives were synthesized by modified Biginelli cyclocondensation reaction catalyzed by MPc as Lewis base. The structures of the synthesized compounds have been successfully characterized by the spectroscopic methods (IR, (1)H NMR, (13C)NMR, UV-Vis, mass spectrometry, elemental analysis and NMR 2D). The influence of substrate/catalyst ratio, solvent was also investigated to find optimal reaction on this synthesis for getting the highest conversion. Different parameters were examined for finding optimal conditions of catalysis. In addition; the compounds 3-11 were investigated for antimicrobial activity. Most of them exhibited important antimicrobial activity. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and anti-HIV activity of novel N-1 side chain-modified analogs of 1-[(2-hydroxyethoxy)methyl]-6-(phenylthio)thymine (HEPT).

PubMed

Pontikis, R; Benhida, R; Aubertin, A M; Grierson, D S; Monneret, C

1997-06-06

A series of 33 N-1 side chain-modified analogs of 1-[(2-hydroxyethoxy)methyl]-6-(phenylthio)thymine (1, HEPT) were synthesized and evaluated for their anti-HIV-1 activity. In particular, the influence of substitution of the terminal hydroxy group of the acyclic structure of HEPT and the structural rigidity of this side chain were investigated. Halo (7, 8), azido (9), and amino (10-15) derivatives were synthesized from HEPT via the p-tosylate derivative 6. Acylation of the primary amine 15 afforded the amido analogs 16-20. The diaryl derivatives 26-29 were prepared by reaction of HEPT, or of the 6-(2-pyridylthio) analog 23, with diaryl disulfides in the presence of tri-n-butylphosphine. Compounds 39-41, in which the N-1 side chain is rigidified by incorporation of an E-configured double bond, were obtained by palladium(0)-catalyzed coupling of several different 6-(arylthio)uracil derivatives (37, 38) with allyl acetates 33. Compounds 13, 40a,c,d,f, and 41, incorporating an aromatic ring at the end of the acyclic side chain, were found to be more potent than the known diphenyl-substituted HEPT analog BPT (2), two of them, 40c,d, being 10-fold more active.

Degradation and Mineralization of Benzohydroxamic Acid by Synthesized Mesoporous La/TiO2

PubMed Central

Luo, Xianping; Wang, Junyu; Wang, Chunying; Zhu, Sipin; Li, Zhihui; Tang, Xuekun; Wu, Min

2016-01-01

Rare earth element La-doped TiO2 (La/TiO2) was synthesized by the sol-gel method. Benzohydroxamic acid was used as the objective pollutant to investigate the photocatalytic activity of La/TiO2. The physicochemical properties of the prepared materials were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, UV-vis diffuse reflectance spectroscopy, specific surface area and porosity, scanning electron microscopy and transmission electron microscopy. As a result, the doping of La could inhibit the crystal growth of TiO2, increase its specific surface area and expand its response to visible light, thus improving its photocatalytic activity. La/TiO2 with the doping ratio of 0.75% calcined at 500 °C, showing the highest photocatalytic activity to degrade benzohydroxamic acid under the irradiation of 300 W mercury lamp. About 94.1% of benzohydroxamic acid with the original concentration at 30 mg·L−1 was removed after 120 min in a solution of pH 4.4 with an La/TiO2 amount of 0.5 g·L−1. Furthermore, 88.5% of the total organic carbon was eliminated after 120 min irradiation. In addition, after four recycling runs, La/TiO2 still kept high photocatalytic activity on the photodegradation of benzohydroxamic acid. The interfacial charge transfer processes were also hypothesized. PMID:27735877

Syntheses, structures, and properties of two new zinc(II) metal-organic frameworks based on flexible 1,6-bis(2-methyl-imidazole-1-yl)hexane ligand

NASA Astrophysics Data System (ADS)

Jin, Jun-Cheng; Fu, Ai-Yun; Li, Dian; Chang, Wen-Gui; Wu, Ju; Yang, Mei; Xie, Cheng-Gen; Xu, Guang-Nian; Cai, An-Xing; Wu, Ai-Hua

2014-11-01

Two new zinc(II) metal-organic compounds of [Zn(ADC)(bimh)]n (1) and [Zn(ADA)(bimh)]n (2) (H2ADC = 1,3-adamantanedicarboxylic acid, H2ADA = 1,3-adamantanediacetic acid, bimh = 1,6-bis(2-methyl-imidazole-1-yl)-hexane, have been structurally characterized by X-ray diffraction analysis. In compound 1, the zinc(II) ions are bridged by ADC and bimh ligands to form a 1D looped chain. In compound 2, the ADA molecules alternately bridge Zn(II) atoms to form infinite chains, and then the 1D chain is connected through the bimh ligand resulting in an undulating infinite two-dimensional (2D) polymeric network. Additionally, TG analysis, XRPD and fluorescent properties for compounds 1 and 2 are also measured and discussed.

Structure elucidation of 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazine, C 23H 18Cl 2N 4OS from synchrotron X-ray powder diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie

The 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazine, C 23H 18Cl 2N 4OS compound was synthesized, as a member of the family of novel potential anticancer agents. The structure of the title compound was characterized by IR, 1H-NMR, mass spectroscopy, and elemental analysis, previously. In this study, the crystal structure of this compound has been determined from synchrotron X-ray powder diffraction data. The crystal structure was solved by simulated annealing and the final structure was achieved by Rietveld refinement method using soft restrains on all interatomic bond lengths and angles. This compound crystallizes in space groupP21,Z= 2, with the unit-cell parametersa= 15.55645(11) Å,b= 8.61693(6) Å,c= 8.56702(6)more » Å,β= 104.3270(4)°, andV= 1112.68(1) Å 3. In the crystal structure, strong C-H∙∙∙πand weak intermolecular hydrogen-bonding interactions link the molecules into a three-dimensional network. The molecules are in a head-to-head arrangement in the unit cell.« less

Preparation of uranium compounds

DOEpatents

Kiplinger, Jaqueline L; Montreal, Marisa J; Thomson, Robert K; Cantat, Thibault; Travia, Nicholas E

2013-02-19

UI.sub.3(1,4-dioxane).sub.1.5 and UI.sub.4(1,4-dioxane).sub.2, were synthesized in high yield by reacting turnings of elemental uranium with iodine dissolved in 1,4-dioxane under mild conditions. These molecular compounds of uranium are thermally stable and excellent precursor materials for synthesizing other molecular compounds of uranium including alkoxide, amide, organometallic, and halide compounds.

Metallic Borides, La 2 Re 3 B 7 and La 3 Re 2 B 5 , Featuring Extensive Boron–Boron Bonding

DOE PAGES

Bugaris, Daniel E.; Malliakas, Christos D.; Chung, Duck Young; ...

2016-01-26

We synthesized La 2Re 3B 7 and La 3Re 2B 5 in single-crystalline form from a molten La/Ni eutectic at 1000°C, in the first example of the flux crystal growth of ternary rare-earth rhenium borides. Both compounds crystallize in their own orthorhombic structure types, with La 2Re 3B 7 (space group Pcca) having lattice parameters a = 7.657(2) Å, b = 6.755(1) Å, and c = 11.617(2) Å, and La 3Re 2B 5 (space group Pmma) having lattice parameters a = 10.809(2) Å, b = 5.287(1) Å, and c = 5.747(1) Å. Furthermore, the compounds possess three-dimensional framework structures thatmore » are built up from rhenium boride polyhedra and boron-boron bonding. La 3Re 2B 5 features fairly common B 2 dumbbells, whereas La 2Re 3B 7 has unique one-dimensional subunits composed of alternating triangular B3 and trans-B4 zigzag chain fragments. Also observed in La 3Re 2B 5 is an unusual coordination of B by an octahedron of La atoms. Electronic band structure calculations predict that La 2Re 3B 7 is a semimetal, which is observed in the electrical resistivity data as measured on single crystals, with behavior obeying the Bloch-Grüneisen model and a room-temperature resistivity ρ300K of ~ 375 μΩ cm. The electronic band structure calculations also suggest that La 3Re 2B 5 is a regular metal.« less

Metallic Borides, La 2 Re 3 B 7 and La 3 Re 2 B 5 , Featuring Extensive Boron–Boron Bonding

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bugaris, Daniel E.; Malliakas, Christos D.; Chung, Duck Young

We synthesized La 2Re 3B 7 and La 3Re 2B 5 in single-crystalline form from a molten La/Ni eutectic at 1000°C, in the first example of the flux crystal growth of ternary rare-earth rhenium borides. Both compounds crystallize in their own orthorhombic structure types, with La 2Re 3B 7 (space group Pcca) having lattice parameters a = 7.657(2) Å, b = 6.755(1) Å, and c = 11.617(2) Å, and La 3Re 2B 5 (space group Pmma) having lattice parameters a = 10.809(2) Å, b = 5.287(1) Å, and c = 5.747(1) Å. Furthermore, the compounds possess three-dimensional framework structures thatmore » are built up from rhenium boride polyhedra and boron-boron bonding. La 3Re 2B 5 features fairly common B 2 dumbbells, whereas La 2Re 3B 7 has unique one-dimensional subunits composed of alternating triangular B3 and trans-B4 zigzag chain fragments. Also observed in La 3Re 2B 5 is an unusual coordination of B by an octahedron of La atoms. Electronic band structure calculations predict that La 2Re 3B 7 is a semimetal, which is observed in the electrical resistivity data as measured on single crystals, with behavior obeying the Bloch-Grüneisen model and a room-temperature resistivity ρ300K of ~ 375 μΩ cm. The electronic band structure calculations also suggest that La 3Re 2B 5 is a regular metal.« less

Structure and cation ordering in La 2UO 6, Ce 2UO 6, LaUO 4, and CeUO 4 by first principles calculations

DOE PAGES

Casillas-Trujillo, Luis; Xu, H.; McMurray, Jake W.; ...

2016-07-06

In the present work, we have used density functional theory (DFT) and DFT+U to investigate the crystal structure and phase stability of four model compounds in the Ln 2O 3-UO 2-UO 3 ternary oxide system: La2UO 6, Ce 2UO 6, LaUO 4, CeUO 4, due to the highly-correlated nature of the f-electrons in uranium. We have considered both hypothetical ordered compounds and compounds in which the cations randomly occupy atomic sites in a fluorite-like lattice. We determined that ordered compounds are stable and are energetically favored compared to disordered configurations, though the ordering tendencies are weak. To model and analyzemore » the structures of these complex oxides, we have used supercells based on a layered atomic model. In the layer model, the supercell is composed of alternating planes of anions and cations. We have considered two different ordering motifs for the cations, namely single species (isoatomic) cation layers versus mixed species cation layers. Energy differences between various ordered cationic arrangements were found to be small. This may have implications regarding radiation stability, since cationic arrangements should be able to change under irradiation with little cost in energy.« less

Synthesis and radical scavenging activity of 6-hydroxyl-4-methylcoumarin and its derivatives

NASA Astrophysics Data System (ADS)

Jumal, Juliana; Ayomide, Adetunji Fridaos

2018-06-01

Four compounds of coumarin derivatives namely 6-hydroxyl-4-methylcoumarin (I), 6-hydroxyl-4-methyl-5-(p-nitrophenyl azocoumarin) (II), 6-hydroxyl-4-methyl-5,7-(bis-p-nitrophenyl azocoumarin) (III) and 6-hydroxyl-4-methyl-5,7-(bis-p-chlorophenyl azocoumarin) (IV) were successfully synthesized. These compounds were prepared by reacting hydroquinone with ethylacetoacetate and selected anilines which are chloro and nitro aniline. All synthesized compounds were characterized by CHN micro-elemental analysis, 1H Nuclear Magnetic Resonance (NMR) and Fourier Transform Infrared (FTIR) spectroscopic methods. The infrared spectra of these compounds exhibited five important stretching vibrations: ʋ(-OH), ʋ(C=O), ʋ(C=C), ʋ(C-O) and ʋ(C-N) at 3441-3359 cm-1, 1604-1632 cm-1, 1581-1496 cm-1, 1331-1225 cm-1, 1251-1109 cm-1, respectively. 1H NMR spectra of these compounds show the presence of proton aromatic, proton methyl and proton pyrone ring with the chemical shift at δH 7.00-8.70 ppm, δH 2.20-2.50 ppm and δH 6.10-6.90 ppm, respectively. CHN analysis results of all compounds are in good agreement with the calculated values. All the synthesized compounds were evaluated for their antioxidant activity using DPPH method and ascorbic acid used as the standard. UV-Vis spectroscopic technique was used to investigate the absorbance of these compounds. Compound (II) shows high antioxidant activities compared to compound (I), (III) and (IV) which show moderate to low activities.

Syntheses of vanadyl and zinc(II) complexes of 1-hydroxy-4,5,6-substituted 2(1H)-pyrimidinones and their insulin-mimetic activities.

PubMed

Yamaguchi, Mika; Wakasugi, Kei; Saito, Ryota; Adachi, Yusuke; Yoshikawa, Yutaka; Sakurai, Hiromu; Katoh, Akira

2006-02-01

Control of the glucose level in the blood plasma has been achieved in vitro and in vivo by administration of vanadium and zinc in form of inorganic salts. It has been shown that elements are poorly absorbed in their inorganic forms and required high doses which have been associated with undesirable side effects. Many researchers, therefore, have focused on metal complexes that were prepared from VOSO(4) or ZnSO(4) and low-molecular-weight bidentate ligands. Seven kinds of 1-hydroxy-4,6-disubstituted and 1-hydroxy-4,5,6-trisubstituted-2(1H)-pyrimidinones were synthesized by reaction of N-benzyloxyurea and beta-diketones and subsequent removal of the protecting group. Six kinds of 1-hydroxy-4-(substituted)amino-2(1H)-pyrimidinones were synthesized by the substitution reaction of 1-benzyloxy-4-(1',2',4'-triazol-1'-yl)-2(1H)-pyrimidinone with various alkyl amines or amino acids. Treatment with VOSO(4) and ZnSO(4) or Zn(OAc)(2) afforded vanadyl(IV) and zinc(II) complexes which were characterized by means of (1)H NMR, IR, EPR, and UV-vis spectroscopies, and combustion analysis. The in vitro insulin-mimetic activity of these complexes was evaluated from 50% inhibitory concentrations (IC(50)) on free fatty acid (FFA) release from isolated rat adipocytes treated with epinephrine. Vanadyl complexes of 4,6-disubstituted-2(1H)-pyrimidinones showed higher insulin-mimetic activities than those of 4,5,6-trisubstituted ones. On the other hand, Zn(II) complexes showed lower insulin-mimetic activities than VOSO(4) and ZnSO(4) as positive controls. It was found that the balance of the hydrophilicity and/or hydrophobicity is important for higher insulin-mimetic activity. The in vivo insulin-mimetic activity was evaluated with streptozotocin (STZ)-induced diabetic rats. Blood glucose levels were lowered from hyperglycemic to normal levels after the treatment with bis(1,2-dihydro-4,6-dimethyl-2-oxo-1-pyrimidinolato)oxovanadium(IV) by daily intraperitoneal injections. The improvement in

Discovery of novel, potent and low-toxicity angiotensin II receptor type 1 (AT1) blockers: Design, synthesis and biological evaluation of 6-substituted aminocarbonyl benzimidazoles with a chiral center.

PubMed

Han, Xiao-Feng; He, Xing; Wang, Miao; Xu, Di; Hao, Li-Ping; Liang, Ai-Hua; Zhang, Jun; Zhou, Zhi-Ming

2015-10-20

Novel angiotensin II receptor type 1 (AT1) blockers bearing 6-substituted carbamoyl benzimidazoles with a chiral center were designed and synthesized as the first step to develop new antihypertensive agents and understand their pharmacodynamic and pharmacokinetic properties. The newly synthesized compounds were tested for their potential ability to displace [(125)I] Sar(1) Ile(8)-Ang II, which was specifically bound to human AT1 receptor. Radioligand binding assays revealed nanomolar affinity in several compounds under study. The IC50 values of nine ligands were higher than those of Losartan. The screening of decreased blood pressure in spontaneous hypertensive rats displayed that compound 8S (IC₅₀ = 5.0 nM) was equipotent with Losartan, whereas compounds 13R (IC₅₀ = 7.3 nM), 14R (IC₅₀ = 6.3 nM), and 14S (IC₅₀ = 3.5 nM) were slightly ahead of Losartan, and the most significant activity was demonstrated by compound 8R (IC₅₀ = 1.1 nM). Candidate 8R was identified for its excellent efficacy in antihypertension and fairly low toxicity based on plasma analyses, toxicology studies, and chronic oral tests. Finally, compound 8R exhibited strong and multiple interactions with target active sites of the theoretical AT1 receptor model in docking study. Copyright © 2015 Elsevier Masson SAS. All rights reserved.

Anticancer activity of synthetic bis(indolyl)methane-ortho-biaryls against human cervical cancer (HeLa) cells.

PubMed

Jamsheena, Vellekkatt; Shilpa, Ganesan; Saranya, Jayaram; Harry, Nissy Ann; Lankalapalli, Ravi Shankar; Priya, Sulochana

2016-03-05

Bis(indolyl)methane appended biaryls were designed, synthesized and evaluated in human cervical cancer cell lines (HeLa) for their anticancer activities and compared against normal rat cardiac myoblasts (H9C2) cells. Compounds 1-12 were synthesized, with variations in one of the phenyl unit, in a single step by condensation of biaryl-2-carbaldehydes with indole in the presence of para-toluenesulfonic acid. Compound 1 exhibited a GI50 value of 11.00 ± 0.707 μM and the derivatives, compounds 4 and 11 showed a GI50 value of 8.33 ± 0.416 μM and 9.13 ± 0.177 μM respectively in HeLa cells and was found to be non-toxic to H9C2 cells up to 20 μM. Furthermore, compounds 1, 4 and 11 induced caspase dependent cellular apoptosis in a concentration-dependent manner, reduced mitochondrial membrane potential, inhibited the cell migration and downregulated the production of MMP-2 and MMP-9 in HeLa cells. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Structure-based virtual screening and characterization of a novel IL-6 antagonistic compound from synthetic compound database.

PubMed

Wang, Jing; Qiao, Chunxia; Xiao, He; Lin, Zhou; Li, Yan; Zhang, Jiyan; Shen, Beifen; Fu, Tinghuan; Feng, Jiannan

2016-01-01

According to the three-dimensional (3D) complex structure of (hIL-6⋅hIL-6R⋅gp 130) 2 and the binding orientation of hIL-6, three compounds with high affinity to hIL-6R and bioactivity to block hIL-6 in vitro were screened theoretically from the chemical databases, including 3D-Available Chemicals Directory (ACD) and MDL Drug Data Report (MDDR), by means of the computer-guided virtual screening method. Using distance geometry, molecular modeling and molecular dynamics trajectory analysis methods, the binding mode and binding energy of the three compounds were evaluated theoretically. Enzyme-linked immunosorbent assay analysis demonstrated that all the three compounds could block IL-6 binding to IL-6R specifically. However, only compound 1 could effectively antagonize the function of hIL-6 and inhibit the proliferation of XG-7 cells in a dose-dependent manner, whereas it showed no cytotoxicity to SP2/0 or L929 cells. These data demonstrated that the compound 1 could be a promising candidate of hIL-6 antagonist.

Syntheses, structural variants and characterization of AInM′S{sub 4} (A=alkali metals, Tl; M′ = Ge, Sn) compounds; facile ion-exchange reactions of layered NaInSnS{sub 4} and KInSnS{sub 4} compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yohannan, Jinu P.; Vidyasagar, Kanamaluru, E-mail: kvsagar@iitm.ac.in

Ten AInM′S{sub 4} (A=alkali metals, Tl; M′= Ge, Sn) compounds with diverse structure types have been synthesized and characterized by single crystal and powder X-ray diffraction and a variety of spectroscopic methods. They are wide band gap semiconductors. KInGeS{sub 4}(1-β), RbInGeS{sub 4}(2), CsInGeS{sub 4}(3-β), TlInGeS{sub 4}(4-β), RbInSnS{sub 4}(8-β) and CsInSnS{sub 4}(9) compounds with three-dimensional BaGa{sub 2}S{sub 4} structure and CsInGeS{sub 4}(3-α) and TlInGeS{sub 4}(4-α) compounds with a layered TlInSiS{sub 4} structure have tetrahedral [InM′S{sub 4}]{sup −} frameworks. On the other hand, LiInSnS{sub 4}(5) with spinel structure and NaInSnS{sub 4}(6), KInSnS{sub 4}(7), RbInSnS{sub 4}(8-α) and TlInSnS{sub 4}(10) compounds with layered structuremore » have octahedral [InM′S{sub 4}]{sup −} frameworks. NaInSnS{sub 4}(6) and KInSnS{sub 4}(7) compounds undergo facile topotactic ion-exchange, at room temperature, with various mono-, di- and tri-valent cations in aqueous medium to give rise to metastable layered phases. - Graphical abstract: NaInSnS{sub 4} and KInSnS{sub 4} compounds undergo, in aqueous medium at room temperature, facile topotactic ion-exchange with mono, di and trivalent cations. Display Omitted - Highlights: • Ten AInM′S{sub 4} compounds with diverse structure types were synthesized. • They are wide band gap semiconductors. • NaInSnS{sub 4} and KInSnS{sub 4} compounds undergo facile topotactic ion-exchange at room temperature.« less

Structure-activity relationship of 5-chloro-2-methyl-3-(1,2,3,6-tetrahydropyridin-4-yl)-1H-indole analogues as 5-HT(6) receptor agonists.

PubMed

Mattsson, Cecilia; Svensson, Peder; Boettcher, Henning; Sonesson, Clas

2013-05-01

To further investigate the structure-activity relationship (SAR) of the 5-hydroxytryptamine type 6 (5-HT6) receptor agonist 5-chloro-2-methyl-3-(1,2,3,6-tetrahydropyridin-4-yl)-1H-indole (EMD386088, 6), a series of 2-methyl-3-(1,2,3,6-tetrahydropyridin-4-yl)-1H-indoles were synthesized, and in vitro affinity to, and functional activity at 5-HT6 receptors was tested. We focused on substituents made at the indole N(1)-, 2- and 5-positions and these were found to not only influence the affinity at 5-HT6 receptors but also the intrinsic activity leading to antagonists, partial agonists and full agonists. In order for a compound to demonstrate potent 5-HT6 receptor agonist properties, the indole N(1) should be unsubstituted, an alkyl group such as 2-methyl is needed and finally halogen substituents in the indole 5-position (fluoro, chloro or, bromo) were essential requirements. However, the introduction of a benzenesulfonyl group at N(1)-position switched the full agonist 6 to be a 5-HT6 receptor antagonist (30). A few compounds within the 2-methyl-3-(1,2,3,6-tetrahydropyridin-4-yl)-1H-indoles were also screened for off-targets and generally they displayed low affinity for other 5-HT subtypes and serotonin transporter protein (SERT). Copyright © 2013 Elsevier Masson SAS. All rights reserved.

Studies on the synthesis and biological activitiy of 6-ethyl-4-aryl-5-methoxycarbonyl-3,4-dihydropyrimidin-2(1H)-ones.

PubMed

Saraç, Selma; Ciftçi, Murat; Zorkun, Inci Selin; Tunç, Ozgül; Erol, Kevser

2007-01-01

6-Ethyl-4-aryl-5-methoxycarbonyl-3,4-dihydropyrimidin-2(1H)-one derivatives (1-10) were synthesized by condensing urea with methyl 3-oxopentanoate and aromatic aldehydes in absol. ethanol using HCl as a catalyst according to the Biginelli reaction. The structures of the compounds were confirmed by spectroscopic and elemental analysis. The calcium channel blocker activities of the compounds were determined by the tests performed on isolated rat ileum and lamb carotid artery. On the isolated rat ileum, compound 2 was found to be more effective at 10(-5) mol/L concentration than nicardipine (CAS 55985-32-5). On the lamb carotid artery compounds 5, 6 and 4, 5, 6 were significantly active at 10(-6) mol/L and 10(-5) mol/L concentrations, respectively.

Microwave Assisted Synthesis of 1-[5-(Substituted Aryl)-1H-Pyrazol-3-yl]-3,5-Diphenyl-1H-1,2,4-Triazole as Antinociceptive and Antimicrobial Agents

PubMed Central

Khanage, Shantaram Gajanan; Mohite, Popat Baban; Pandhare, Ramdas Bhanudas; Raju, S. Appala

2014-01-01

Purpose: An efficient technique has been developed for microwave assisted synthesis of 1-[5-(substituted aryl)-1H-pyrazol-3-yl]-3,5-diphenyl-1H-1,2,4-triazole as antinociceptive and antimicrobial agents. Methods: The desired compounds (S1-S10) were synthesized by the microwave irradiation via cyclization of formerly synthesized chalcones of 3,5-diphenyl-1H-1,2,4-triazole and hydrazine hydrate in mild acidic condition. All newly synthesized compounds were subjected to study their antinociceptive and antimicrobial activity. The analgesic potential of compounds was tested by acetic acid induced writhing response and hot plate method. The MIC values for antimicrobial activity were premeditated by liquid broth method. Results: The compounds S1, S2, S4, S6 and S10 were found to be excellent peripherally acting analgesic agents when tested on mice by acetic acid induced writhing method and compounds S3, S6 and S1 at dose level of 100 mg/kg were exhibited superior centrally acting antinociceptive activity when tested by Eddy’s hot plate method. In antimicrobial activity compound S10 found to be broad spectrum antibacterial agent at MIC value of 15.62 µg/ml and compound S6 was exhibited antifungal potential at 15.62 µg/mL on both fungal strains. Conclusion: Some novel pyrazoles clubbed with 1,2,4-triazole derivatives were synthesized and evaluated as possible antimicrobial, centrally and peripherally acting analgesics. PMID:24511473

Discovery of novel indole derivatives as allosteric inhibitors of fructose-1,6-bisphosphatase.

PubMed

Bie, Jianbo; Liu, Shuainan; Li, Zhanmei; Mu, Yongzhao; Xu, Bailing; Shen, Zhufang

2015-01-27

A series of novel indole derivatives was designed and synthesized as inhibitors of fructose-1,6-bisphosphatase (FBPase). The most potent compound 14c was identified with an IC50 value of 0.10 μM by testing the inhibitory activity against recombinant human FBPase. The structure-activity relationships were investigated on the substitution at 4- and 5-position of the indole scaffold. The binding interactions of the title compounds at AMP binding site of FBPase were predicted using CDOCKER algorithm. Copyright © 2014 Elsevier Masson SAS. All rights reserved.

Novel Energetic Compounds Based on 3-Methyl-1,2,5-Oxadiazole 2-Oxide

NASA Astrophysics Data System (ADS)

Xu, Zhen; Yang, Hongwei; Cheng, Guangbin

2018-01-01

Two derivatives of 3-methyl-1,2,5-oxadiazole 2-oxide, (E) 4-methyl-1,2,5-oxadiazole-3-carboxaldehyde 5-oxide (2,4,6-trinitrophenyl)hydrazone (1) and 2,2,2-trinitroethyl 4-methyl-1,2,5-oxadiazole-3-carboxylate 5-oxide (2), were designed, synthesized, and fully characterized. The structures of the new compounds were confirmed by single-crystal X-ray analysis. Physicochemical and energetic properties including density, thermal stability, and sensitivity were investigated, and energetic properties (e.g., detonation velocities and detonation pressures) were calculated using EXPLO5 code. The results indicated that compound 1 exhibits positive heat of formation of 448.0 kJ mol-1 and acceptable sensitivities (IS: 20 J, FS: 280 N). In addition, compound 2 possesses low melting point (99.92°C), moderate decomposition temperature (183.67°C), good detonation performances (D: 8430 m s-1; P: 31.5 GPa), and lower sensitivities (IS: 18 J; FS: 220 N), which suggest 2 has the potential to be melt-cast explosive.

Synthesis of novel fluorinated chalcones derived from 4‧-morpholinoacetophenone and their antiproliferative effects

NASA Astrophysics Data System (ADS)

Kurşun Aktar, Bedriye Seda; Oruç-Emre, Emine Elçin; Demirtaş, Ibrahim; Yaglioglu, Ayse Sahin; Guler, Caglar; Adem, Sevki; Karaküçük Iyidoğan, Ayşegül

2017-12-01

The fluorinated chalcones were synthesized by Claisen-Schmidt condensation between 4‧-morpholineacetophenone and various fluorinated benzaldehydes in the presence of NaOH in methanol. The synthesized compounds [1-7] were evaluated their antiproliferative activity against HeLa and C6 cell lines. Among them, compounds 4 and 5 were determined to have anticancer activity against HeLa cells line (IC50 values of 7.74 and 6.10 μg/mL, respectively). The anticancer activity results were shown that compounds 3, and 6 had inhibitory against C6 cells (IC50 values of 12.80 and 4.16 μg/mL, respectively). The compounds 1 and 2 had high antiproliferative activity with non-cytotoxicity. All of the new compounds, except for compound 4 showed inhibition against the human isozyme hCA I with IC50 in the range of 0.5-1,16 mM. Pyruvate kinase M2 (PKM2) was effectively inhibited by compound 4 with IC50 = 26 μM.

Effect of Zn doping on structural, magnetic and dielectric properties of LaFeO{sub 3} synthesized through sol–gel auto-combustion process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bhat, Irshad; Husain, Shahid, E-mail: s.husain@lycos.com; Khan, Wasi

2013-11-15

Graphical abstract: - Highlights: • We have synthesized the samples of LaFe{sub 1−x}Zn{sub x}O{sub 3} (0 ≤ x ≤ 0.3) using sol–gel auto-combustion process. • The doping of Zn{sup 2+} hugely enhances the dielectric constant (ε′) and it shows a colossal value. • The parent compound LaFeO{sub 3} does not show any relaxation peak, but the substitution of Zn at Fe{sup 3+} site brings the relaxation in the system. • The system shows a peak behavior thereby giving the Debye like dipolar relaxation response. - Abstract: We have studied the structural and dielectric properties of nano-crystalline LaFe{sub 1−x}Zn{sub x}O{sub 3}more » (0 ≤ x ≤ 0.3) pervoskite samples synthesized through sol–gel auto-combustion technique. X-ray diffraction and FTIR spectroscopy are used to confirm the single phase characteristics. Microstructural features are investigated using scanning electron microscope and compositional analysis is performed through energy dispersive spectroscopy. The average grain sizes, calculated from the Scherrer formula, lie in the range below 30 nm. The hysteresis (M-H) curves display a weak magnetic order and a shift in the hysteresis loops. Dielectric response has been discussed, in the framework of “universal dielectric response” model. The value of dielectric constant (ε′) increases drastically on Zn doping. The dielectric loss factor (ε″) shows Debye like dipolar relaxation behavior. The observed peaks in loss factor (ε″) are attributed to the fact that a strong correlation between the conduction mechanism and the dielectric behavior exists in ferrites.« less

Antifouling potential of Nature-inspired sulfated compounds

NASA Astrophysics Data System (ADS)

Almeida, Joana R.; Correia-da-Silva, Marta; Sousa, Emília; Antunes, Jorge; Pinto, Madalena; Vasconcelos, Vitor; Cunha, Isabel

2017-02-01

Natural products with a sulfated scaffold have emerged as antifouling agents with low or nontoxic effects to the environment. In this study 13 sulfated polyphenols were synthesized and tested for antifouling potential using the anti-settlement activity of mussel (Mytilus galloprovincialis) plantigrade post-larvae and bacterial growth inhibition towards four biofilm-forming bacterial strains. Results show that some of these Nature-inspired compounds were bioactive, particularly rutin persulfate (2), 3,6-bis(β-D-glucopyranosyl) xanthone persulfate (6), and gallic acid persulfate (12) against the settlement of plantigrades. The chemical precursors of sulfated compounds 2 and 12 were also tested for anti-settlement activity and it was possible to conclude that bioactivity is associated with sulfation. While compound 12 showed the most promising anti-settlement activity (EC50 = 8.95 μg.mL-1), compound 2 also caused the higher level of growth inhibition in bacteria Vibrio harveyi (EC20 = 12.5 μg.mL-1). All the three bioactive compounds 2, 6, and 12 were also found to be nontoxic to the non target species Artemia salina (<10% mortality at 250 μM) and Vibrio fischeri (LC50 > 1000 μg.mL-1). This study put forward the relevance of synthesizing non-natural sulfated small molecules to generate new nontoxic antifouling agents.

Antifouling potential of Nature-inspired sulfated compounds

PubMed Central

Almeida, Joana R.; Correia-da-Silva, Marta; Sousa, Emília; Antunes, Jorge; Pinto, Madalena; Vasconcelos, Vitor; Cunha, Isabel

2017-01-01

Natural products with a sulfated scaffold have emerged as antifouling agents with low or nontoxic effects to the environment. In this study 13 sulfated polyphenols were synthesized and tested for antifouling potential using the anti-settlement activity of mussel (Mytilus galloprovincialis) plantigrade post-larvae and bacterial growth inhibition towards four biofilm-forming bacterial strains. Results show that some of these Nature-inspired compounds were bioactive, particularly rutin persulfate (2), 3,6-bis(β-D-glucopyranosyl) xanthone persulfate (6), and gallic acid persulfate (12) against the settlement of plantigrades. The chemical precursors of sulfated compounds 2 and 12 were also tested for anti-settlement activity and it was possible to conclude that bioactivity is associated with sulfation. While compound 12 showed the most promising anti-settlement activity (EC50 = 8.95 μg.mL−1), compound 2 also caused the higher level of growth inhibition in bacteria Vibrio harveyi (EC20 = 12.5 μg.mL−1). All the three bioactive compounds 2, 6, and 12 were also found to be nontoxic to the non target species Artemia salina (<10% mortality at 250 μM) and Vibrio fischeri (LC50 > 1000 μg.mL−1). This study put forward the relevance of synthesizing non-natural sulfated small molecules to generate new nontoxic antifouling agents. PMID:28205590

An alkaline tin(II) halide compound Na{sub 3}Sn{sub 2}F{sub 6}Cl: Synthesis, structure, and characterization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gong, Pifu; University of the Chinese Academy of Sciences, Beijing 100049; Luo, Siyang

A new alkali tin(II) halide compound, Na{sub 3}Sn{sub 2}F{sub 6}Cl, is synthesized by hydrothermal method. This compound crystallizes trigonally in space group of R-3c (167), and processes a zero-dimensional (0D) structure consisted of Na{sup +} cations, Cl{sup −} anions and the isolated [SnF{sub 3}]{sup -} trigonal pyramids in which the stereochemically active 5s{sup 2} lone pair electrons are attached to the Sn{sup 2+} cations. Interestingly, the [SnF{sub 3}]{sup −} trigonal pyramids are parallel arranged in the a-b plane, while oppositely arranged in line with rotation along the c- axis. Moreover, the energy bandgap, thermal stability and electronic structure of Na{submore » 3}Sn{sub 2}F{sub 6}Cl are characterized and the results reveal that this compound has and indirect bandgap of 3.88 eV and is stable under 270 °C. - Graphical abstract: A zero-dimensional alkaline tin halide compound, Na{sub 3}Sn{sub 2}F{sub 6}Cl, is synthesized by hydrothermal method. Interestingly, both the anions and cations coordinating polyhedra exhibit order arranged with the [SnF{sub 3}]{sup -} trigonal pyramids rotating along the c- axis.« less

Synthesis of Substituted 2,3,5,6-tetraarylbenzo(1,2-b:5,4-b')difurans

NASA Technical Reports Server (NTRS)

Abdul-Aziz, Mahmoud; Auping, Judith V.; Meador, Michael A.

1995-01-01

A series of substituted 2,3,5,6-tetraarylbenzo(l,2-b:5,4-b')difurans 1 was synthesized. This synthesis is based upon the photocyclization of 2,5-dibenzoylresorcinol dibenzyl ethers to the corresponding tetrahydrobenzo(1,2-b:5,4-b')difurans. Treatment of the photoproducts with methanesulfonyl chloride in pyridine afforded 1 in overall yields ranging from 30-72%. A number of these compounds have high fluorescence quantum yields (of phi(sub f) = 0.76-0.90), and their fluorescence spectra exhibit large solvatochromic shifts. These compounds may be suitable for use as fluorescent probes.

Phase equilibria in the La–Mg–Ge system at 500 °C and crystal structure of the new ternary compounds La{sub 11}Mg{sub 2}Ge{sub 7} and LaMg{sub 3−x}Ge{sub 2}

DOE Office of Scientific and Technical Information (OSTI.GOV)

De Negri, S., E-mail: serena.denegri@unige.it; Solokha, P.; Skrobańska, M.

2014-10-15

The whole 500 °C isothermal section of the La–Mg–Ge ternary system was constructed. The existence and crystal structure of three ternary compounds were confirmed: La{sub 2+x}Mg{sub 1−x}Ge{sub 2} (τ{sub 2}, P4/mbm, tP10–Mo{sub 2}FeB{sub 2}, 0≤x≤0.25), La{sub 4}Mg{sub 5}Ge{sub 6} (τ{sub 3}, Cmc2{sub 1}, oS60–Gd{sub 4}Zn{sub 5}Ge{sub 6}) and La{sub 4}Mg{sub 7}Ge{sub 6} (τ{sub 4}, C2/m, mS34, own structure type). Five novel compounds were identified and structurally characterized: La{sub 11}Mg{sub 2}Ge{sub 7} (τ{sub 1}, P4{sub 2}/ncm, tP88-8, own structure type, a=1.21338(5), c=1.57802(6) nm), LaMg{sub 3−x}Ge{sub 2} (τ{sub 5}, P3{sup ¯}1c, hP34-0.44, own structure type, x=0.407(5), a=0.78408(4), c=1.45257(7) nm), La{sub 6}Mg{sub 23}Gemore » (τ{sub 6}, Fm3{sup ¯}m, cF120–Zr{sub 6}Zn{sub 23}Si, a=1.46694(6) nm), La{sub 4}MgGe{sub 10−x} (τ{sub 7}, x=0.37(1), C2/m, mS60-1.46, own structure type, a=0.88403(8), b=0.86756(8), c=1.7709(2) nm, β=97.16°(1) and La{sub 2}MgGe{sub 6} (τ{sub 8}, Cmce, oS72–Ce{sub 2}(Ga{sub 0.1}Ge{sub 0.9}){sub 7}, a=0.8989(2), b=0.8517(2), c=2.1064(3) nm). Disordering phenomena were revealed in several La–Mg–Ge phases in terms of partially occupied sites. The crystal structures of La{sub 11}Mg{sub 2}Ge{sub 7} and LaMg{sub 3−x}Ge{sub 2} are discussed in details. The latter is a √3a×√3a×2c superstructure of the LaLi{sub 3}Sb{sub 2} structure type; the symmetry reduction scheme is shown in the Bärnighausen formalism terms. - Graphical abstract: La–Mg–Ge isothermal section at 500 °C and group–subgroup relation between the LaLi{sub 3}Sb{sub 2} (parent type) and LaMg{sub 3−x}Ge{sub 2} (derivative) structures. - Highlights: • Novel La−Mg−Ge compounds structure determination from X-ray single crystal data. • Disordering phenomena as common features of the studied germanides. • Bärnighausen formalism as a useful tool for accurate structure determination. • Full isothermal section of the

Acute Dermal Toxicity of 1,2,3,4-Tetrahydro-6-Methyl-(3-Methyl-1-Oxo-2-Butenyl) Quinoline (CHR6) in Rabbits.

DTIC Science & Technology

1983-09-01

la ,lb). Edema was associated with the first two days of redness and was * . seen along the abrasions on the back. Only 1 of 12 animals exposed to...Toxicology Group, Division of Research Support ARA ZWR UI UBR Letterman Army Institute of Research Project 3MI6,77OA871 Presidio of San Francisco, CA...abraded areas. This compound should be exposed to further toxicological testing for human use potential as an insect repellent Co~ de Name for 1.2.3.4

New carbocyclic N(6)-substituted adenine and pyrimidine nucleoside analogues with a bicyclo[2.2.1]heptane fragment as sugar moiety; synthesis, antiviral, anticancer activity and X-ray crystallography.

PubMed

Tănase, Constantin I; Drăghici, Constantin; Cojocaru, Ana; Galochkina, Anastasia V; Orshanskaya, Jana R; Zarubaev, Vladimir V; Shova, Sergiu; Enache, Cristian; Maganu, Maria

2015-10-01

New nucleoside analogues with an optically active bicyclo[2.2.1]heptane skeleton as sugar moiety and 6-substituted adenine were synthesized by alkylation of 6-chloropurine intermediate. Thymine and uracil analogs were synthesized by building the pyrimidine ring on amine 1. X-ray crystallography confirmed an exo-coupling of the thymine to the ring and an L configuration of the nucleoside analogue. The library of compounds was tested for their inhibitory activity against influenza virus A∖California/07/09 (H1N1)pdm09 and coxsackievirus B4 in cell culture. Compounds 13a and 13d are the most promising for their antiviral activity against influenza, and compound 3c against coxsackievirus B4. Compounds 3b and 3g were tested for anticancer activity. Copyright © 2015 Elsevier Ltd. All rights reserved.

Crystal growth and characterization of the CMR compound La 1.2(Sr,Ca) 1.8Mn 2O 7

NASA Astrophysics Data System (ADS)

Velázquez, M.; Haut, C.; Hennion, B.; Revcolevschi, A.

2000-12-01

High-quality centimeter-sized single crystals of La 1.2Sr 1.8- yCa yMn 2O 7 (0.0⩽ y⩽0.2) were successfully grown using a floating zone method associated with an image furnace. We present the growth conditions together with a characterization of the single crystals by means of optical and electron microscopy, EDX and ICP⧸AES analysis, DTA-TGA measurements and redox titration, X-ray powder diffraction, Laue X-ray back-reflection and neutron diffraction. We also stress the main aspects of the complex thermodynamical and kinetic behaviors of these compounds.

Investigation of structural and electrical properties of La{sub 0.7}(Ba{sub 1-x}Ca{sub x}){sub 0.3}MnO{sub 3} compounds by sol-gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Winarsih, Suci; Kurniawan, Budhy, E-mail: bkuru07@gmail.com; Manaf, Azwar

2016-06-17

In this paper, we explored structural and electrical properties of La{sub 0.7}(Ba{sub 1-x}Ca{sub x}){sub 0.3}MnO{sub 3} (x = 0; 0.03; and 0.05) compounds. The general structure of perovskite manganites is AMnO{sub 3} (A= trivalent rare earth with divalent ion-doped). Average A-site cation size, external pressure, and the variance of the cation size σ{sup 2} are one of many factors that affected to magneto-transport properties of manganites as reported by others. In this work we focus only on the electrical properties in La{sub 0.7}Ba{sub 0.3}MnO{sub 3} Ca-doped compound which may influence crystal structure resulting resistivity phenomena under magnetic field influence. Allmore » samples were synthesized by sol-gel method from which fine powders were obtained. The X-ray powder diffraction pattern of powder materials shows that all samples are fully crystalline with a rhombohedral structure. Rietveld refinement shows that the presence of calcium has changed some crystal structural parameters such lattice parameter, Mn–O bond length, and Mn–O–Mn angles. The electrical resistivity of all synthesized materials investigated by four point probe method using Cryogenic Magnet in the temperature range of 50-300 K under influence a magnetic field shows resistivity temperature dependent. In fact presence of calcium has reduced the resistivity. It might occure because it has made an enhancement in the mobility of hopping electrons. The magnetic external field causes the resistivity decreased for all samples because host spin align by delocalizing the charge carries so electron itinerant through the lattice suggested by other authors. Both calcium dopant concentration and the applied external magnetic field shows strong correlation in reduction of resistivity.« less

4,6-Diaryl/heteroarylpyrimidin-2(1H)-ones as a new class of xanthine oxidase inhibitors.

PubMed

Shukla, Shiwani; Kumar, Dinesh; Ojha, Ritu; Gupta, Manish K; Nepali, Kunal; Bedi, Preet M S

2014-07-01

A series of 4,6-diaryl/heteroarylpyrimidones was synthesized employing silica-supported fluoroboric acid under solvent-free conditions in a microwave reactor. The catalytic influence of HBF4-SiO2 was investigated in detail to optimize the reaction conditions. The synthesized compounds were evaluated for in vitro xanthine oxidase (XO) inhibitory activity for the first time. Structure-activity relationship analyses are also presented. Among the synthesized compounds, VA-5, -9, -10, -12, -22, -23, and -25 were the active inhibitors with IC50 values ranging from 6.45 to 13.46 µM. Compound VA-25 with a pyridinyl ring as ring A and a thiophenyl ring as ring B emerged as the most potent XO inhibitor (IC50 = 6.45 µM) in comparison to allopurinol (IC50 = 12.24 µM). Some of the important interactions of VA-25 with the amino acid residues of the active site of XO were figured out by molecular modeling studies. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Novel 1,5-diphenyl-6-substituted 1H-pyrazolo[3,4-d]pyrimidin-4(5H)-ones induced apoptosis in RKO colon cancer cells.

PubMed

Malki, Ahmed; Ashour, Hayam M A; Elbayaa, Rasha Y; Issa, Doaa A E; Aziz, Hassan A; Chen, Xiaozhuo

2016-12-01

Novel 1,5-diphenyl-6-substituted-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-ones were synthesized and characterized. All compounds were screened for their anti-proliferative activities in five different cancer cell lines. The results showed that compounds 7a and 7b comprising aminoguanidino or guanidino moiety at position 6 inhibited proliferation of RKO colon cancer cells with IC50 of 8 and 4 μM, respectively. Compounds 7a and 7b induced apoptosis in RKO cells, which was confirmed by TUNEL and annexin V-FITC assays. Flow cytometric analysis indicated that compounds 7a and 7b arrested RKO cells in the G1 phase and the most active compound 7b increased levels of p53, p21, Bax, ERK1/2 and reduced levels of Bcl2 and Akt. Compound 7b also activates release of cytochrome c, which is consistent with activation of caspase-9. Additionally, compound 7b increased caspase-3 activity and cleaved PARP-1 in RKO cells. Collectively, these findings could establish a molecular basis for the development of new anti-cancer agents.

Synthesized of 2,7 dihydroxyxanthone from xanthone and antimalarial activities

NASA Astrophysics Data System (ADS)

Amanatie; Jumina; Mustofa; Hanafi

2018-03-01

The purpose of the research is to synthesize 2,7-di-hydroxyxanthone compounds from xanthone and to evaluate antiplasmodial against activities. The synthesize of 2,7-di-hydroxyxanthone compounds worked with chromatogramphy methods including Thin Layer Chromatography (TLC), Vacuum Liquid Chromatography (VLC). A compound structures were determined based on the spectroscopic evidences including, Infrared (IR), one dimension (1-D) and two dimension (2-D) Nuclear Magnetic Resonance (NMR) spectra and comparison the spectroscopy data with related data from references. The biological properties of compounds are evaluated towards antiplasmodial against activity. The result of the product was obtained as white solid in 63.49% yield. The IR spectrum showed the absorption at 3433 cm-1 Which was reinforced with a sharp attack at 1087cm-1 indicating the stretching of OH, while the stretching of aromatic C=C appeared at 1620 cm-1. The 1H-NMR (500MHz, and DMSO –d6) spectrum showed that the aryl protons appeared in the region of δ12.98 ppm. In this region, there were 2 singlet at δH 12.98 ppm (1H, 2-OH) and (1H,7-OH) and shows the presence of two OH groups. Based on spectroscopy analyses, it could be started that the reaction of 2.7 di-aminoxanthone with NaNO2/HCl and H3PO4 produced 2.7-di-hydroxyxanthone. In vitro antiplasmodial assay of the product synthesized 2,7 di-hydroxyxanthones against. Falciparum strain of 3D7 showed that the IC50 values of 2,7-di-hydroxy xanthone, were 0.31 μg/mL, respectively.

Electrochemical performances of co-substituted (La and Li) LiLa{sub x−y}Li{sub y}Ni{sub 1−x}O{sub 2} cathode materials for rechargeable lithium-ion batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohan, P.; Paruthimal Kalaignan, G., E-mail: pkalaignan@yahoo.com

2013-09-01

Graphical abstract: - Highlights: • LiLa{sub x−y}Li{sub x}Ni{sub 1−x}O{sub 2} powders were prepared by a sol–gel method at 600 °C for 10 h. • LiLa{sub x−y}Li{sub x}Ni{sub 1−x}O{sub 2} powder materials had well defined layer structure, and no impurities. • LiLa{sub 0.10}Li{sub 0.10}Ni{sub 0.80}O{sub 2} crystallite size was reduced compared with those of LiNiO{sub 2}. • Li/LiPF{sub 6}/LiLa{sub x−y}Li{sub x}Ni{sub 1−x}O{sub 2} cells were of high charge/discharge capacity, with columbic efficiency at 25 °C and 45 °C. • LiLa{sub 0.10}Li{sub 0.10}Ni{sub 0.80}O{sub 2} good cyclic stability, rate capability and better 45 °C. - Abstract: Co-substituted LiLa{sub x−y}Li{sub y}Ni{sub 1−x}O{sub 2}more » cathode materials were synthesized by sol–gel method using aqueous solutions of metal nitrates and tartaric acid as chelating agent at 600 °C for 10 h. The structure and electrochemical properties of the synthesized materials were characterized by using XRD, SEM, EDAX, TEM, cyclic voltammetry, charge/discharge and electrochemical impedance spectroscopy. XRD studies revealed a well defined layer structure and a linear variation of lattice parameters with the addition of lanthanum and lithium confirmed phase pure compounds in a rhombohedral structure. TEM and SEM analysis shows that LiLa{sub 0.10}Li{sub 0.10}Ni{sub 0.80}O{sub 2} has smaller particle size and regular morphological structure with narrow size distribution than those of LiNiO{sub 2}. Variations of dual mixing and hexagonal ordering with the substituted elements have enhanced the charge/discharge capacities at both room (25 °C) and elevated temperatures (45 °C), respectively. LiLa{sub 0.10}Li{sub 0.10}Ni{sub 0.80}O{sub 2} had high charge/discharge capacity, low irreversible capacity and better elevated temperature performance.« less

Structure determination of two structural analogs, named 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) by synchrotron X-ray powder diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie

Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C 23H 16F 2N 4S) (1) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C 23H 16ClFN 4S) (2), have been designed and synthesized as cytotoxic agents. The compounds were characterized by infrared, proton nuclear magnetic resonance, mass spectral data, elemental analysis and X-ray powder diffraction. The present study comprises spectral data and crystal structures of these novel compounds determined from synchrotron X-ray powder diffraction data. The structure solutions were obtained by simulated annealing. The final structures were achieved by Rietveld refinement using soft restraints for all bond lengths, bond angles, and planar groups. Both compounds crystallize in space groupmore » $$P\\bar 1$$,Z= 2, with the unit-cell parametersa= 6.37433(9),b= 11.3641(2),c= 14.09115(19) Å,α= 80.1740(8)°,β= 85.1164(8)°,γ= 80.9831(10)°,V= 991.55(3) Å 3of compound (1) anda= 6.53736(6),b= 11.55725(15),c= 14.01373(13) Å,α= 80.3323(7)°,β= 84.8939(6)°,γ= 79.3954(8)°,V= 1024.08(2) Å 3of compound (2). Structural analyses reveal that the title compounds are isostructural.« less

Detailed investigation of thermal and electron transport properties in strongly correlated compound Ce6Pd12In5 and its nonmagnetic analog La6Pd12In5

NASA Astrophysics Data System (ADS)

Falkowski, M.; Krychowski, D.; Strydom, A. M.

2016-11-01

An in-depth study of thermal and electron transport properties including thermal conductivity κ(T), thermoelectric power S(T), and electrical resistivity ρ(T) of the heavy fermion Kondo lattice Ce6Pd12In5 and its nonmagnetic reference compound La6Pd12In5 is presented. The absolute κ(T) value of Ce6Pd12In5 is smaller that than of La6Pd12In5, which indicates that conduction electron-4f electron scattering has a large impact on the reduction of thermal conductivity. The isolated 4f electron contributions to the electrical resistivity ρ 4 f (T), electronic thermal resistivity displayed in the form W e l , 4 f (T) .T, and thermoelectric power S 4 f (T) reveal a low- and high-temperature -lnT behaviour characteristic of Kondo systems with strong crystal-electric field (CEF) interactions. The analysis of phonon scattering processes of lattice thermal conductivity κph(T) in (Ce, La)6Pd12In5 was performed over the whole accessible temperature range according to the Callaway model. In the scope of a theoretical approach based on the perturbation type calculation, we were able to describe our experimental data of ρ 4 f (T) and W e l , 4 f (T) .T by using the model incorporating simultaneously the Kondo effect in the presence of the CEF splitting, as it is foreseen in the framework of the Cornut-Coqblin and Bhattacharjee-Coqblin theory. Considering the fact that there are not many cases of similar studies at all, we also show the numerical calculations of temperature-dependent behaviour of spin-disorder resistivity ρs(T), magnetic resistivity ρ 4 f (T), and occupation number ⟨ N i ⟩ due to the various types of degeneracy of the ground state multiplet of Ce 3 + (J = 5/2).

1-(substituted benzyl)-3,4,5,6-tetrahydro-2(1H)-pyrimidones: a series with stimulant and depressant activities.

PubMed

Ellis, K O; Schwan, T J; Wessels, F L; Miles, N J

1980-10-01

A series of 1-(substituted benzyl)-3,4,5,6-tetrahydro-2(1H)-pyrimidones was synthesized primarily by catalytic hydrogenation of the corresponding 1-(substituted benzyl)-2(1H)-pyrimidone. The pharmacological evaluation of these compounds in mice revealed a unique profile that included evidence of CNS stimulation and depression within the series and in the same compounds. Some members of this series induced signs of only CNS stimulation, some compounds caused signs of only CNS depression and skeletal muscle relaxation, and some caused signs of both stimulation and depression in the same animal. This apparent dual activity was assessed further in mice with antidepressant tests based on tetrabenazine antagonism and with antianxiety/anticonvulsant tests on the antagonism of a number of convulsants. The 4-chloro-, 4-fluoro-, 4-bromo-, and 3,4-dichlorobenzyl compounds exhibited antidepressant and antianxiety activities in the same dose range. Among these four compounds, the 3,4-dichlorobenzyl compound possessed the lowest antitetrabenazine (17 mg/kg po) and antipentylenetetrazol (23 mg/kg po) ED50 values. The 4-fluoro compound antagonized tetrabenazine-, pentylenetetrazol-, and isoniazid-induced tonic convulsions in the same dose range (congruent to 50 mg/kg po).

Heat capacity and magnetocaloric effect in manganites (La 1- yEu y) 0.7Pb 0.3MnO 3 ( y:0.2; 0.6)

NASA Astrophysics Data System (ADS)

Kartashev, A. V.; Flerov, I. N.; Volkov, N. V.; Sablina, K. A.

2010-03-01

Heat capacity and intensive magnetocaloric effect (MCE) in manganites (La 1- yEu y) 0.7Pb 0.3MnO 3 [ y=0.2; 0.6] (LEPM) were investigated by means of adiabatic calorimeter. The heat capacity anomaly as well as the values of both the intensive (Δ TAD) and the extensive (Δ SMCE) MCE were found to decrease upon increased replacement of La with nonmagnetic Eu. However, because of widening of the MCE peaks, the LEPM compounds show the relative cooling power, RCP/Δ H, comparable to other solid solutions of manganites. Owing to strong effect of Eu→La substitution on the Curie temperature, LEPM might have potential as the solid state refrigerants in multi-element cooling apparatus operating in a wide temperature range.

Effect of Sm substitution on magnetic and magnetocaloric properties of La0.7-xSmxBa0.3MnO3 (0 ≤ x ≤ 0.2) compounds

NASA Astrophysics Data System (ADS)

Modi, Anchit; Gaur, N. K.

2017-11-01

In the present paper we have studied the effect of Sm doping on the magnetic and magnetocaloric properties of La0.7-xSmxBa0.3MnO3 (0 ≤ x ≤ 0.2) compounds. These sample have been synthesized by conventional solid state reaction method. The analysis of synthesized samples by X-ray diffraction showed that the formation of single phase compositions and doping of La3+ by Sm3+ ion converted the chemical structure form rhombohedral (R-3C) to orthorhombic (Imma). The magnetic study measurement specified that the ferromagnetic double exchange interaction is weakened with increasing Sm content as a consequence of the curie temperature (Tc) shift in lower temperature from 340 K for x = 0, 290 K for x = 0.1 and 225 K for x = 0.2 compounds. Using the Banerjee's criterion plots, it is found that the phase transition for all samples in the second-order. All reported compounds exhibit a maximum and large magneto-caloric effect near the Curie temperature (Tc). The magnitude of the maximum magnetic entropy change is found to be decrease with increasing of Sm doping content i.e. 4.39 J/kg K for x = 0, 4.22 J/kg K for x = 0.1 and 2.48 J/kg K for x = 0.2 in applied field change of 5T. The trend of large entropy change and the convenient adjustment of the Curie temperature make these oxides useful for magnetic refrigeration in an extended high and low temperature even at near room temperature.

Ionothermal synthesis and structural transformation targeted by ion exchange in metal-1,3,5-benzenetricarboxylate compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Qing-Qing; State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002; Liu, Bing

Ionothermal reactions of 1,3,5-benzenetricarboxylate acid (H{sub 3}BTC) and Ni(NO{sub 3}){sub 2}, Co(NO{sub 3}){sub 2} and Cu(NO{sub 3}){sub 2} gave two discrete 32-membered ring-like allomers, [M{sub 2}(HBTC){sub 2}(NH{sub 2}CONH{sub 2}){sub 2}(H{sub 2}O){sub 4}]·3H{sub 2}O (M=Ni(1), Co(2)) and one layered [Cu{sub 2}(BTC)Cl(H{sub 2}O){sub 4}] (3). The weak interactions in 1 can be deconstructed to some degree in ion exchange by exploring the factors of divalent and trivalent metal species, metal concentration and soaking time, which are demonstrated by PXRD and N{sub 2} absorption. Cu{sup 2+} has the highest N{sub 2} adsorbance when soaking with 1, and 1 can keep structure stable whenmore » Cu{sup 2+} below 0.16 mol L{sup −1} and the soaking time within 24d. As Cu{sup 2+} beyond 0.16 mol L{sup −1} and the soaking time beyond 24d, the structure of compound 1 starts to transform with the crystal morphology from clear pale green to opaque blue. Ionothermal reactions of compound 1 with different Cu{sup 2+} amounts obtained Ni{sup 2+}-Cu{sup 2+} hetero complexes, whose PXRD patterns are similar to that of 3 and EDS indicates Cu{sup 2+}% increases with Cu{sup 2+} additions and close to 100% as Cu{sup 2+} being 1.6 mmol. It suggests that 3 is a controlled product and Cu{sup 2+} can transform discrete compound 1 into 2D compound 3. - Graphical abstract: Three compounds were synthesized through ionothermal reactions. The weak interactions in compound 1 can be deconstructed by ion exchange and discrete compound 1 can be transformed into layered compound 3. - Highlights: • Two discrete ring-like and one layered compounds were ionothermally synthesized. • Metal species, metal concentration and soaking time deconstruct the H-bondings in 1. • 1 can be transformed to 3 through ionothermal reaction, otherwise forbidden.« less

Proteomic Characterization of Plasmid pLA1 for Biodegradation of Polycyclic Aromatic Hydrocarbons in the Marine Bacterium, Novosphingobium pentaromativorans US6-1

PubMed Central

Yun, Sung Ho; Choi, Chi-Won; Lee, Sang-Yeop; Lee, Yeol Gyun; Kwon, Joseph; Leem, Sun Hee; Chung, Young Ho; Kahng, Hyung-Yeel; Kim, Sang Jin; Kwon, Kae Kyoung; Kim, Seung Il

2014-01-01

Novosphingobium pentaromativorans US6-1 is a halophilic marine bacterium able to degrade polycyclic aromatic hydrocarbons (PAHs). Genome sequence analysis revealed that the large plasmid pLA1 present in N. pentaromativorans US6-1 consists of 199 ORFs and possess putative biodegradation genes that may be involved in PAH degradation. 1-DE/LC-MS/MS analysis of N. pentaromativorans US6-1 cultured in the presence of different PAHs and monocyclic aromatic hydrocarbons (MAHs) identified approximately 1,000 and 1,400 proteins, respectively. Up-regulated biodegradation enzymes, including those belonging to pLA1, were quantitatively compared. Among the PAHs, phenanthrene induced the strongest up-regulation of extradiol cleavage pathway enzymes such as ring-hydroxylating dioxygenase, putative biphenyl-2,3-diol 1,2-dioxygenase, and catechol 2,3-dioxygenase in pLA1. These enzymes lead the initial step of the lower catabolic pathway of aromatic hydrocarbons through the extradiol cleavage pathway and participate in the attack of PAH ring cleavage, respectively. However, N. pentaromativorans US6-1 cultured with p-hydroxybenzoate induced activation of another extradiol cleavage pathway, the protocatechuate 4,5-dioxygenase pathway, that originated from chromosomal genes. These results suggest that N. pentaromativorans US6-1 utilizes two different extradiol pathways and plasmid pLA1 might play a key role in the biodegradation of PAH in N. pentaromativorans US6-1. PMID:24608660

Synthesis, spectroscopic investigations (FT-IR, NMR, UV-Vis, and TD-DFT), and molecular docking of (E)-1-(benzo[d][1, 3]dioxol-6-yl)-3-(6-methoxynaphthalen-2-yl)prop-2-en-1-one

NASA Astrophysics Data System (ADS)

Therasa Alphonsa, A.; Loganathan, C.; Athavan Alias Anand, S.; Kabilan, S.

2017-02-01

The compound (E)-1-(benzo [d] [1, 3] dioxol-6-yl)-3-(6-methoxy naphthalen-2-yl) prop-2-en-1-one (AKN) was synthesized and characterized by FT-IR, NMR, and UV-Vis spectrometer. The optimized molecular geometry, bond lengths, bond angles, atomic charges, harmonic vibrational wave numbers and intensities of vibrational bonds of the title compound have been investigated by Time dependent- Density Functional Theory (TD-DFT) using a standard B3LYP method with 6-31 G (d, p) basis set available in the Gaussian 09W package. 1H and 13C NMR chemical shifts of the molecule were calculated using Gauge-independent atomic orbital method (GIAO). Experimental excitation energies of the molecules were matched with the theoretically calculated energies. The atomic charge distributions of the various atoms present in the AKN were obtained by Mulliken charge population analysis. The Molecular Electrostatic Potential (MEP) analysis reveals the sites for electrophilic attack and nucleophilic reactions in the molecule. The difference between the observed and scaled frequencies was small. The HOMO to LUMO transition implies an electron density transfer. The intramolecular contacts have been interpreted using Natural Bond Orbital (NBO) analysis. The calculation results were applied to simulate spectra of the title compound, which show excellent agreement with observed spectra. To provide information about the interactions between human cytochrome protein and the novel compound theoretically, docking studies were carried out using Schrödinger software.

Uncommon and Emissive {[Au2(C3H6NS2)2][Au(C3H6NS2)2]2(PF6)2} Mixed Au+ and Au3+ Pseudotetranuclear Crystalline Compound: Synthesis, Structural Characterization, and Optical Properties.

PubMed

Langaro, Ana P; Souza, Ana K R; Morassuti, Claudio Y; Lima, Sandro M; Casagrande, Gleison A; Deflon, Victor M; Nunes, Luiz A O; Da Cunha Andrade, Luis H

2016-11-23

An uncommon emissive pseudotetranuclear compound, {[Au 2 (C 3 H 6 NS 2 ) 2 ][Au(C 3 H 6 NS 2 ) 2 ] 2 (PF 6 ) 2 }, was synthesized and characterized in terms of its structure and optical properties. The synthesis produced a crystalline compound composed of four gold atoms with two different oxidation states (Au + and Au 3+ ) in the same crystalline structure. The title complex belonged to a triclinic crystalline system involving the centrosymmetric P1̅ space group. X-ray diffractometry and vibrational spectroscopy (infrared, Raman, and SERS) were used for structural characterization of the new crystal. The vibrational spectroscopy techniques supported the X-ray diffraction results and confirmed the presence of bonds including Au-Au and Au-S. Optical characterization performed using UV-vis spectroscopy showed that under ultraviolet excitation, the emissive crystalline complex presented characteristic broad luminescent bands centered at 420 and 670 nm.

Two new coordination polymers constructed by naphthalene-1,4-dicarboxylic acid and 2,4-diamino-6-methyl-triazine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Yamin, E-mail: liyamin@henu.edu.cn; Xiao, Changyu; Zhang, Xudong

2013-08-15

Two new transition metal coordination complexes, ([MnO(nda)](H{sub 2}dmt)(H{sub 2}O)){sub n} (1), [Ag{sub 5}(nda){sub 2.5}(dmt)]{sub n} (2), (H{sub 2}nda=naphthalene-1,4-dicarboxylic acid, dmt=2,4-diamine-6-methyl-1,3,5-triazine) have been hydrothermally synthesized by the reactions of H{sub 2}nda and dmt with the homologous MnCl{sub 2}·4H{sub 2}O and AgNO{sub 3}, respectively, and characterized by single-crystal X-ray diffraction, IR spectra, elemental analysis, thermogravimetric analysis (TGA). The compound 1 exhibits a 3D network comprising 1D metal chain (MnO(CO{sub 2}){sub 2}){sub n} connected by the ligand nda{sup 2−}, featuring a four-connected uninodal diamond -like topology. In compound 2, it is firstly observed that decanuclear silver units as secondary building units to constructmore » 3D network by the ligands dmt and nda{sup 2−}, with a rare 2-nodal (3,8)-connected tfz-d topology ((4{sup 3}){sub 2}(4{sup 6}.6{sup 18}.8{sup 4})). The interactions within each Mn(II)—Mn(II) pair of compound 1 are antiferromagnetic (g=2.07, J=−1.42(1) cm{sup −1}, zj′=−0.73(2) cm{sup −1}). In addition, compound 2 exhibits photoluminescent property at about 472 nm (λ{sub ex}=394 nm). - Graphical abstract: Two new transition metal coordination complexes 1–2 have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction, IR spectra, elemental analysis thermogravimetric analysis (TGA). Highlights: • The compound 1 exhibits a 3D network with four-connected uninodal diamond-like topology. • The first 3D network of 2 with a rare tfz-d topology consists of decanuclear silver clusters as secondary building units. • The magnetic measurement indicates the compound 1 shows antiferromagnetic interactions. • The photoluminescent property of 2 has been measured.« less

Synthesis and fluorescence emission properties of 1,3,6,8-tetraarylpyrenes

NASA Astrophysics Data System (ADS)

Hu, Jian-Yong; Feng, Xing; Tomiyasu, Hirotsugu; Seto, Nobuyuki; Rayhan, Ummey; Elsegood, Mark R. J.; Redshaw, Carl; Yamato, Takehiko

2013-09-01

Three types of stable pyrene-based highly fluorescence (blue) compounds, 1-, 1,6-bis, 1,8-bis and 1,3,6,8-tetrakis(7-tert-butylpyrenyl)pyrenes and 1,3,6,8-tetrakis[9,9-bis(3-methylbutyl)-9H-fluoren-2-yl]pyrene, were successfully synthesized via a Pd/Cu-catalysed Suzuki cross-coupling reaction of the corresponding bromopyrenes with 7-tert-butyl-1-pyrenylboronic ester or 2-[9,9-bis(3-methylbutyl)-9H-fluoren-2-yl]-4,4,5,5-tetramethyl[1,3,2]dioxaborolane, respectively. All compounds have good solubility in common organic solvents and high thermal stability with melting points up to 270 °C; the exceptions are the isomeric 1,6-bis-, and 1,8-bispyrenyl-substituted pyrenes. All products show high extinction coefficients of absorption (λmax ≈ 349-396 nm) and high quantum yields (λmax ≈ 432-465 nm; Φf ≈ 0.75-0.99) in dichloromethane solution, and emit strong fluorescence in the visible region ranging from deep-blue to pure-blue on increasing the number of substituents. This data suggests that such systems have promise as blue emitters in organic light-emitting device (OLED) applications (OLED = organic light emitting diode). Crystal structures were determined for 1,3,6,8-tetrakis [9,9-bis(3-methylbutyl)-9H-fluoren-2-yl] pyrene and 1,3,6,8-tetrakis(4-methoxyphenyl)pyrene.

Novel compounds TAD-1822-7-F2 and F5 inhibited HeLa cells growth through the JAK/Stat signaling pathway.

PubMed

Yang, Tianfeng; Shi, Xianpeng; Kang, Yuan; Zhu, Man; Fan, Mengying; Zhang, Dongdong; Zhang, Yanmin

2018-07-01

Cervical carcinoma remains the second most common malignancy with a high mortality rate among women worldwide. TAD-1822-7-F2 (F2) and TAD-1822-7-F5 (F5) are novel compounds synthesized on the chemical structure of taspine derivatives, and show an effective suppression for HeLa cells. Our study aims to confirm the potential targets of F2 and F5, and investigate the underlying mechanism of the inhibitory effect on HeLa cells. In this study, Real Time Cell Analysis and crystal violet staining assay were conducted to investigate the effect of F2 and F5 on HeLa cells proliferation. And the analytical methods of surface plasmon resonance and quartz crystal microbalance were established and employed to study the interaction between F2 and F5 and potential target protein JAK2, suggesting that both compounds have strong interaction with the JAK2 protein. Western blot analysis, immunofluorescence staining study and PCR was conducted to investigate the molecules of JAK/Stat signaling pathway. Interestingly, F2 and F5 showed diverse regulation for signaling molecules because of their different chemical structure. F2 increased the expression of JAK2 and downregulated the level of P-JAK1 and P-JAK2, and decreased P-Stat3 (Ser727). While F5 could increase the expression of JAK2 and naturally decrease the phosphorylation of JAK1 and Tyk2, and decreased the expression of P-Stat6. Moreover, F2 and F5 showed the same downregulation on the P-Stat3 (Tyr705). Therefore, F2 and F5 could target the JAK2 protein and prevent the phosphorylation of JAKs to suppress the phosphorylation of the downstream effector Stats, which suggested that F2 and F5 have great potential to be the inhibitors of the JAK/Stat signaling pathway. Copyright © 2018 Elsevier Masson SAS. All rights reserved.

Li1.2Mn0.6Ni0.1Co0.1O2 microspheres constructed by hierarchically arranged nanoparticles as lithium battery cathode with enhanced electrochemical performance

NASA Astrophysics Data System (ADS)

Remith, P.; Kalaiselvi, N.

2014-11-01

Novel lithium-rich layered Li1.2Mn0.6Ni0.1Co0.1O2 microspheres containing hierarchically arranged and interconnected nanostructures have been synthesized by a combination of template-free co-precipitation and solid-state methods. The in situ formed γ-MnO2 spherical template upon co-precipitation gets sacrificed during the course of solid-state fusion of cobalt, nickel and lithium precursors to produce the title compound in the form of microspheres constructed by nanoparticles as building blocks. Porous and hollow microspheres of Li1.2Mn0.6Ni0.1Co0.1O2 are formed out of the spontaneous aggregation of nanoparticles, obtained from the custom-designed synthesis protocol. The growth mechanism of Li1.2Mn0.6Ni0.1Co0.1O2 spheres could be understood in terms of the Kirkendall effect and Ostwald ripening. The nanocrystalline Li1.2Mn0.6Ni0.1Co0.1O2 compound is obtained as a solid solution consisting of rhombohedral R3&cmb.macr;m and monoclinic C2/m group symmetries, as evidenced by XRD, Raman spectra and HRTEM equipped with FFT and STEM. The currently synthesized Li1.2Mn0.6Ni0.1Co0.1O2 cathode exhibits an appreciable discharge capacity of 242 mA h g-1 at a current density of 50 mA g-1, due to the synergistic effect of the capacity obtained from the rhombohedral and monoclinic phases.Novel lithium-rich layered Li1.2Mn0.6Ni0.1Co0.1O2 microspheres containing hierarchically arranged and interconnected nanostructures have been synthesized by a combination of template-free co-precipitation and solid-state methods. The in situ formed γ-MnO2 spherical template upon co-precipitation gets sacrificed during the course of solid-state fusion of cobalt, nickel and lithium precursors to produce the title compound in the form of microspheres constructed by nanoparticles as building blocks. Porous and hollow microspheres of Li1.2Mn0.6Ni0.1Co0.1O2 are formed out of the spontaneous aggregation of nanoparticles, obtained from the custom-designed synthesis protocol. The growth mechanism of Li1

Stereoselective synthesis, spectral and antimicrobial studies of some cyanoacetyl hydrazones of 3-alkyl-2,6-diarylpiperidin-4-ones

NASA Astrophysics Data System (ADS)

Velayutham Pillai, M.; Rajeswari, K.; Vidhyasagar, T.

2014-11-01

A series of novel cyanoacetyl hydrazones of 3-alkyl-2,6-diarylpiperidin-4-ones were synthesized stereoselectively and characterized by IR, Mass, 1H NMR, 13C NMR, 1H-1H COSY and 1H-13C COSY spectra. The stereochemistry of the synthesized compounds was established using NMR spectra. Antimicrobial screening of the synthesized compounds revealed their antibacterial and antifungal potencies. Growth inhibition of Enterobacter Aerogenes by compound 15 was found to be superior to the standard drug.

A new class of anticonvulsants possessing 6 Hz psychomotor seizure test activity: 2-(1H-benzotriazol-1-yl)-N'-[substituted] acetohydrazides.

PubMed

Kumar, Praveen; Tripathi, Laxmi

2012-05-01

A series of 2-(1H-Benzotriazol-1-yl)-N'-[substituted]acetohydrazides were designed & synthesized keeping in view the structural requirement of pharmacophore and evaluated for anticonvulsant activity and neurotoxicity. The new compounds were characterized using FT-IR, 1H NMR, mass spectral data and elemental analysis. The anticonvulsant activity of the titled compounds was assessed using the 6 Hz psychomotor seizure test. The neurotoxicity was assessed using the rotorod method. The most active compound of the series was N'-[4-(1,3-Benzodioxol-5-yloxy)benzylidene]-2-(1H-benzotriazol-1-yl)acetohydrazide (BTA 9), which showed good activity with 75 % protection (3/4, 0.5 h) at a dose of 100 mg/kg in mice. All the compounds exhibited no neurotoxicity. A computational study was carried out for calculation of pharmacophore pattern and prediction of pharmacokinetic properties. Titled compounds have also exhibited good binding properties with epilepsy molecular targets such as glutamate, GABA (A) delta, GABA (A) alpha-1 receptors and Na/H exchanger, in Lamarckian genetic algorithm based flexible docking studies.

Synthesis and Biological Evaluation of Substituted N-[3-(1H-Pyrrol-1-yl)methyl]-1,2,5,6-tetrahydropyridin-1-yl]benzamide/ benzene Sulfonamides as Anti-Inflammatory Agents

PubMed Central

Gangapuram, Madhavi; Mazzio, Elizabeth; Eyunni, Suresh; Soliman, Karam F. A.; Redda, Kinfe K.

2014-01-01

The pharmacological activities of tetrahydropyridine (THP) derivatives are dependent on the substituent ring moiety. In this study, we investigate the anti-inflammatory activities of 12 newly synthesized substituted N-[3-(1H-pyrrol-1-yl)methyl]-1,2,5,6-tetrahydrobenzamide/benzene sulfonamides (9a–l) in murine BV-2 microglial cells. All compounds were initially screened for attenuation of nitric oxide (NO) production in lipopolysaccharide (LPS) (1 μg/mL)-activated microglial cells. The data show that only SO2-substituted THPs were effective at sub-lethal concentrations (IC50 values of 12.92 μM (9i), 14.64 μM (9j), 19.63 μM (9k)) relative to L-N6-(1-iminoethyl)lysine positive control (IC50 = 3.1 μM). The most potent SO2-substituted compound (9i) also blocked the LPS-inducible nitric oxide synthase (iNOS) and attenuated the release of several cytokines including IL-1α, IL-10, and IL-6. These findings establish the moderate immunomodulating effects of SO2-substituted THP derivatives. PMID:24585402

Structural, vibrational and NMR spectroscopic investigations of newly synthesized 3-((ethylthio)(4-nitrophenyl)methyl)-1H-indole

NASA Astrophysics Data System (ADS)

Bhat, Sheeraz Ahmad; Dar, Ajaz A.; Ahmad, Shabbir; Khan, Abu T.

2017-10-01

The compound 3-((ethylthio)(4-nitrophenyl)methyl)-1H-indole was synthesized at room temperature through one-pot three-component reaction from 1H-indole, 4-nitrobenzaldehyde, and ethanethiol using hydrated ferric sulfate as a Lewis acid catalyst. The structure was characterised by single crystal XRD, FTIR (4000-400 cm-1), FT-Raman (4000-50 cm-1) and 1H and 13C NMR analysis. The compound crystallizes in the monoclinic with volume 3238.3(9) Å3. The experimental vibrational data find the theoretical support through anharmonic frequency calculations using DFT/B3LYP level of theory in combination with 6-31G(d,p) basis set. It is observed that the predicted geometry well reproduces the XRD structural parameters. The experimental 1H and 13C NMR spectra in CDCl3 solvent and the simulated spectra predicted using gauge independent atomic orbital (GIAO) approach are also found in agreement with each other. HOMO-LUMO, MEP, atomic charges and various other thermodynamic and NLO properties of the title molecule are also reported in this paper.

Monodentate phosphine substitution in [Pd(κ3-dppf)(PR3)][BF4]2 (dppf = 1,1'-bis(diphenylphosphino)ferrocene) compounds.

PubMed

Cabrera, K D; Rowland, A T; Szarko, J M; Diaconescu, P L; Bezpalko, M W; Kassel, W S; Nataro, C

2017-05-02

The ligand 1,1'-bis(diphenylphosphino)ferrocene (dppf) is commonly employed in a variety of catalytic systems. There are a variety of coordination modes known for dppf, the least studied being the κ 3 coordination mode, in which both phosphorus atoms and the iron atom of dppf interact with another metal center. One such compound is the previously reported [Pd(κ 3 -dppf)(PPh 3 )] 2+ . A series of related compounds, [Pd(κ 3 -dppf)(P(p-C 6 H 4 R) 3 )] 2+ (R = OCH 3 , CH 3 , F and CF 3 ), has been synthesized and characterized. The X-ray crystal structure of [Pd(dppf)(P(p-C 6 H 4 F) 3 )][BF 4 ] 2 was determined. Electrochemical and computational studies indicate that the electron donor ability of the P(p-C 6 H 4 R) 3 ligands influences the properties of these compounds. Substitution reactions of the P(p-C 6 H 4 R) 3 ligands have been examined, and, in general, the more electron donating P(p-C 6 H 4 R) 3 ligands completely replace the less electron donating ones. The kinetics of the reaction of [Pd(κ 3 -dppf)(P(p-C 6 H 4 F) 3 )] 2+ with P(p-C 6 H 4 OCH 3 ) 3 indicate that the reaction proceeds through a dissociative mechanism, contrary to the associative substitutions prevalent in square planar palladium(ii) chemistry.

Synthesis and biological evaluation of some 4-(1H-indol-3-yl)-6-phenyl-1,2,3,4-tetrahydropyrimidin-2-ones/thiones as potent anti-inflammatory agents.

PubMed

Amir, Mohammad; Javed, Sadique Akhtar; Kumar, Harish

2008-12-01

Twelve new 4-(1H-indol-3-yl)-6-phenyl-1,2,3,4-tetrahydropyrimidin-2-ones/thiones (7-18) have been synthesized by reacting 1-aryl-3-(1H-indol-3-yl)-2-propen-1-one with urea and thiourea in ethanolic potassium hydroxide. Their structures have been confirmed by IR, 1H NMR and mass spectral data. The compounds were tested for their anti-inflammatory activity. Test results revealed that compounds showed 49.5 to 70.7% anti-inflammatory activity where-as the standard drug ibuprofen showed 86.4% activity at the same oral dose. Four compounds, 4-(1H-indol-3-yl)-6-(4-chlorophenyl)-1,2,3,4-tetrahydropyrimidin-2-one (8), 4-(1H-indol-3-yl)-6-(4-methylphenyl)-1,2,3,4-tetrahydropyrimidin-2-one (10), 4-(1H-indol-3-yl)-6-(4-chlorophenyl)-1,2,3,4-tetrahydropyrimidin-2-thione (14), 4-(1H-indol-3-yl)-6-(4-methylphenyl)-1,2,3,4-tetrahydropyrimidin-2-thione (16), that showed significant anti-inflammatory activity were selected to study their ulcerogenic and lipid peroxidation activities. All tested compounds showed significant reduction in the ulcerogenic potential and lipid peroxidation compared to the standard drug ibuprofen.

Oxygen permeation and stability of La 0.4Ca 0.6Fe 1-xCo xO 3-δ ( x = 0, 0.25, 0.5) membranes

NASA Astrophysics Data System (ADS)

Diethelm, S.; Van herle, J.; Middleton, P. H.; Favrat, D.

Three perovskite-type compounds of composition La 0.4Ca 0.6Fe 1- xCo xO 3- δ ( x=0, 0.25 and 0.5) were investigated for use as oxygen separation membranes for the partial oxidation (POX) of methane to syngas. Special attention was given to the question of their stability in real operating conditions. A permeation set-up was specially designed to measure oxygen fluxes through these materials when placed in a strong pO 2 gradient. It also facilitated testing the long-term stability of the specimen. Permeation measurements performed in an air/argon gradient between 800 and 1000 °C showed that the highest fluxes were obtained with the highest content of cobalt (La 0.4Ca 0.6Fe 0.5Co 0.5O 3- δ ≅ La 0.4Ca 0.6Fe 0.75Co 0.25O 3- δ > La 0.4Ca 0.6FeO 3- δ). In addition, comparison between the fluxes of samples of different thickness gave clear evidence of surface limitations in the oxygen transport. The long-term stability test showed opposite trends: only the two lowest Co containing compounds ( x=0 and 0.25) sustained an air/(Ar+H 2) gradient over more than 600 h. The other ( x=0.5) broke shortly after the introduction of H 2. In the presence of H 2, the oxygen flux was increased by a factor 10 compared to Ar and reached 0.83 μmol/cm 2 s for La 0.4Ca 0.6Fe 0.75Co 0.25O 3- δ at 900 °C. Post-operation SEM examination of the cross-section and both surfaces revealed that the surface exposed to H 2 had started to decompose resulting in the formation of a thin porous layer but the bulk of the material remained unchanged.

Discovery of novel and potent small-molecule inhibitors of NO and cytokine production as antisepsis agents: synthesis and biological activity of alkyl 6-(N-substituted sulfamoyl)cyclohex-1-ene-1-carboxylate.

PubMed

Yamada, Masami; Ichikawa, Takashi; Ii, Masayuki; Sunamoto, Mie; Itoh, Katsumi; Tamura, Norikazu; Kitazaki, Tomoyuki

2005-11-17

To develop a new therapeutic agent for sepsis, screening of the Takeda chemical library was carried out using mouse macrophages stimulated with lipopolysaccharide (LPS) to identify a new class of small-molecule inhibitors of inflammatory mediator production. The lead compound 5a was discovered, from which a series of novel cyclohexene derivatives I bearing a sulfamoyl and ester group were designed, synthesized and tested for their inhibitory activity against nitric oxide (NO) production. Derivatives I were synthesized by the coupling of sulfonyl chlorides and anilines with concomitant double bond migration in the presence of triethylamine, and phenyl ring substitution and modification of the ester and cyclohexene moieties were carried out. Among the compounds synthesized, ethyl (6R)-6-[N-(2-chloro-4-fluorophenyl)sulfamoyl]cyclohex-1-ene-1-carboxylate [(R)-(+)-5n, TAK-242] was found to exhibit the most potent suppressive activity for the production of not only NO but also inflammatory cytokines, such as tumor necrosis factor-alpha (TNF-alpha) and interleukin-6 (IL-6) induced by LPS-stimulated mouse macrophages with IC50 values of 1.8, 1.9 and 1.3 nM, respectively. It shows marked beneficial effects in vivo also. Intravenous administration of (R)-(+)-5n at doses of 0.1 mg/kg or more suppressed the production of NO and various cytokines [TNF-alpha, IL-6 and IL-1beta] in the mouse endotoxin shock model. Furthermore, it protected mice from death dose-dependently and all mice survived at a dose of 3 mg/kg. The minimum effective dose to protect mice from lethality in this model was 0.3 mg/kg, which was consistent with those for inhibitory effects on the production of NO and cytokines. Compound (R)-(+)-5n is currently undergoing clinical trials for the treatment of sepsis.

A critical review of both the synthesis approach and the receptor profile of the 8-chloro-1-(2',4'-dichlorophenyl)-N-piperidin-1-yl-1,4,5,6-tetrahydrobenzo[6,7]cyclohepta[1,2-c]pyrazole-3-carboxamide and analogue derivatives.

PubMed

Lazzari, Paolo; Distinto, Rita; Manca, Ilaria; Baillie, Gemma; Murineddu, Gabriele; Pira, Marilena; Falzoi, Matteo; Sani, Monica; Morales, Paula; Ross, Ruth; Zanda, Matteo; Jagerovic, Nadine; Pinna, Gérard Aimè

2016-10-04

8-Chloro-1-(2',4'-dichlorophenyl)-N-piperidin-1-yl-1,4,5,6-tetrahydrobenzo[6,7]cyclohepta[1,2-c]pyrazole-3-carboxamide 9a was discovered as potent and selective CB1 antagonist by part of our group few years ago. In particular it was reported to have an affinity towards the CB1 cannabinoid receptor (CB1R), expressed as Ki, of 0.00035 nM. Nevertheless significantly divergent data were reported for the same compound from other laboratories. To unequivocally define the receptor profile of 9a, we have critically reviewed both its synthesis approach and binding data. Here we report that, in contrast to our previously reported data, 9a showed a Ki value for CB1R in the order of nanomolar rather than of fentomolar range. The new determined receptor profile of 9a was also ascertained for analogue derivatives 9b-i, as well as for 12. Moreover, the structural features of the synthesized compounds necessary for CB1R were investigated. Amongst the novel series, effects on CB1R intrinsic activity was highlighted due to the substituents at the position 3 of the pyrazole ring of the 1,4,5,6-tetrahydrobenzo[6,7]cyclohepta[1,2-c]pyrazole scaffold. Although the cannabinoid receptor profile of 9a was reviewed in this work, the relevance of this compound in CB1R antagonist based drug discovery is confirmed. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

Effect of microstructure on the thermoelectric performance of La{sub 1−x}Sr{sub x}CoO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Viskadourakis, Z.; Department of Mechanical and Manufacturing Engineering, University of Cypruss, 75 Kallipoleos Avenue, P.O. Box 20537, 1678 Nicosia; Athanasopoulos, G.I.

We present a case where the microstructure has a profound effect on the thermoelectric properties of oxide compounds. Specifically, we have investigated the effect of different sintering treatments on La{sub 1−x}Sr{sub x}CoO{sub 3} samples synthesized using the Pechini method. We found that the samples, which are dense and consist of inhomogeneously-mixed grains of different size, exhibit both higher Seebeck coefficient and thermoelectric figure of merit than the samples, which are porous and consist of grains with almost identical size. The enhancement of Seebeck coefficient in the dense samples is attributed to the so-called “energy-filtering” mechanism that is related to themore » energy barrier of the grain boundary. On the other hand, the thermal conductivity for the porous compounds is significantly reduced in comparison to the dense compounds. It is suggested that a fine-manipulation of grain size ratio combined with a fine-tuning of porosity could considerably enhance the thermoelectric performance of oxides. - Graphical abstract: The enhancement of the dimensionless thermoelectric figure ZT of merit is presented for two equally Sr-doped LaCoO3 compounds, possessing different microstructure, indicating the effect of the latter to the thermoelectric performance of the La{sub 1−x}Sr{sub x}CoO{sub 3} solid solution. - Highlights: • Electrical and thermal transport properties are affected by the microstructure in La{sub 1−x}Sr{sub x}CoO{sub 3} polycrystalline materials. • Coarse/fine grain size distribution enhances the Seebeck coefficient. • Porosity reduces the thermal conductivity in La{sub 1−x}Sr{sub x}CoO{sub 3} polycrystalline samples. • The combination of large/small grain ratio distribution with the high porosity may result to the enhancement of the thermoelectric performance of the material.« less

The effect of newly synthesized progesterone derivatives on apoptotic and angiogenic pathway in MCF-7 breast cancer cells.

PubMed

Yahya, Shaymaa M M; Abdelhamid, Abdou O; Abd-Elhalim, Mervat M; Elsayed, Ghada H; Eskander, Emad F

2017-10-01

Due to its high potency and selectivity, anticancer agents consisting of combined molecules have gained great interests. The current study introduces newly synthesized progesterone derivatives of promising anticancer effect. Moreover, the pro-apoptotic and anti-angiogenic effects of these compounds were studied extensively. Several thiazole, pyridine, pyrazole, thiazolopyridine and pyrazolopyridine progesterone derivatives were synthesized. The structure of the novel progesterone derivatives was elucidated and confirmed using the analytical and spectral data. This novel derivatives were tested for their cytotoxic effect against human breast cancer cells (MCF-7) using neutral red uptake assay. Tested compounds showed anticancer activity against MCF-7 cancer cell line in the descending order of 7>2>3>8>6>9>4. The expression levels of Bcl-2, survivin, CCND1, CDC2, P53 and P21, VEGF, Hif-1α, MMP-2, MMP-9, Ang-1, Ang-2, and FGF-1 genes were investigated using QRT-PCR (Quantitative real time-polymerase chain reaction). The study clarified that compounds 2, 3, 4, 6, 7, 8 and 9 showed significant pro-apoptotic effect through the down regulation of Bcl-2., besides, survivin and CCND1 expression levels were down regulated by compounds 3, 4, 6, 7, 8, 9. However, Compound 4 may exert this pro-apoptotic effect through the up-regulation of P53 gene expression. On the other hand, the anti-angiogenic effect of these newly synthesized derivatives was due to their down regulation of VEGF, Ang-2, MMP-9 and FGF-1; and the up-regulation of HIF-1α and ang-1. This study recommended promising pro-apoptotic and anti-angiogenic anticancer agents acting through the regulation of key regulators of apoptosis, cell cycle genes, and pro-angiogenic genes. Copyright © 2017 Elsevier Inc. All rights reserved.

Structural, dielectric and impedance studies of polycrystalline La0.6Dy0.2Ca0.2MnO3

NASA Astrophysics Data System (ADS)

Nandan, K. R.; Kumar, A. Ruban

2017-05-01

Polycrystalline materials of Dy doped La1-xCaxMnO3 were prepared by Sol-Gel technique using citric acid as a chelating agent at 900°C. The compound was analyzed by powder X-ray diffraction technique and confirmed to be single phased orthorhombic perovskite structure with space group Pnma. From the dielectric and impedance studies confirmed the existence of dielectric relaxation and presence of space charge were observed from the dielectric constant and impedance plots respectively and confirms the existence of relaxation due to oxygen vacancy. Cole-cole plot confirms the presence of dielectric relaxation and grain contribution in the synthesized sample.

Structural variation from heterometallic cluster-based 1D chain to heterometallic tetranuclear cluster: Syntheses, structures and magnetic properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Shu-Hua, E-mail: zsh720108@163.com; Zhao, Ru-Xia; Li, He-Ping

Using the solvothermal method, we present the comparative preparation of ([Co{sub 3}Na(dmaep){sub 3}(ehbd)(N{sub 3}){sub 3}]·DMF){sub n} (1) and [Co{sub 2}Na{sub 2}(hmbd){sub 4}(N{sub 3}){sub 2}(DMF){sub 2}] (2), where Hehbd is 3-ethoxy-2-hydroxy-benzaldehyde, Hhmbd is 3-methoxy-2-hydroxy-benzaldehyde, and Hdmaep is 2-dimethylaminomethyl-6-ethoxy-phenol, which was synthesized by an in-situ reaction. Complexes 1 and 2 were characterized by elemental analysis, IR spectroscopy, and X-ray single-crystal diffraction. Complex 1 is a novel heterometallic cluster-based 1-D chain and 2 is a heterometallic tetranuclear cluster. The (Co{sub 3}{sup II}Na) and (Co{sub 2}{sup II}Na{sub 2}) cores display dominant ferromagnetic interaction from the nature of the binding modes through μ{sub 1,1,1}-N{sub 3}{supmore » –} (end-on, EO). - Graphical abstract: Two novel cobalt complexes have been prepared. Compound 1 consists of tetranuclear (Co{sub 3}{sup II}Na) units, which further formed a 1-D chain. Compound 2 is heterometallic tetranuclear cluster. Two complexes display dominant ferromagnetic interaction. - Highlights: • Two new heterometallic complexes have been synthesized by solvothermal method. • The stereospecific blockade of the ligands in the synthesis system seems to be the most important synthetic parameter. • The magnetism studies show that 1 and 2 exhibit ferromagnetic interactions. • Complex 1 shows slowing down of magnetization and not blocking of magnetization.« less

Structure-5-HT/D2 Receptor Affinity Relationship in a New Group of 1-Arylpiperazynylalkyl Derivatives of 8-Dialkylamino-3,7-dimethyl-1H-purine-2,6(3H,7H)-dione.

PubMed

Żmudzki, Paweł; Satała, Grzegorz; Chłoń-Rzepa, Grażyna; Bojarski, Andrzej J; Kazek, Grzegorz; Siwek, Agata; Gryboś, Anna; Głuch-Lutwin, Monika; Wesołowska, Anna; Pawłowski, Maciej

2016-10-01

In our previous papers, we have reported that some 8-amino-1,3-dimethyl-1H-purine-2,6(3H,7H)-dione derivatives possessed high affinity and displayed agonistic, partial agonistic, or antagonistic activity for serotonin 5-HT 1A and dopamine D 2 receptors. In order to examine further the influence of the substituent in the position 8 of the purine moiety and the influence of the xanthine core on the affinity for serotonin 5-HT 1A , 5-HT 2A , 5-HT 6 , 5-HT 7 , and dopamine D 2 receptors, two series of 1-arylpiperazynylalkyl derivatives of 8-amino-3,7-dimethyl-1H-purine-2,6(3H,7H)-dione were synthesized. All the final compounds were investigated in in vitro competition binding experiments for the serotonin 5-HT 1A , 5-HT 2A , 5-HT 6 , 5-HT 7 , and dopamine D 2 receptors. The structure-affinity relationships for this group of compounds were discussed. For selected compounds, the functional assays for the 5-HT 1A and D 2 receptors were carried out. The results of the assays indicated that these groups of derivatives possessed antagonistic activity for 5-HT 1A receptors and agonistic, partial agonistic, or antagonistic activity for D 2 receptors. In total, 26 new compounds were synthesized, 20 of which were tested in in vitro binding experiments and 5 were tested in in vitro functional assays. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Design, synthesis, and characterization of (1-(4-aryl)- 1H-1,2,3-triazol-4-yl)methyl, substituted phenyl-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylates against Mycobacterium tuberculosis

PubMed Central

Venugopala, Katharigatta N; Dharma Rao, G B; Bhandary, Subhrajyoti; Pillay, Melendhran; Chopra, Deepak; Aldhubiab, Bandar E; Attimarad, Mahesh; Alwassil, Osama Ibrahim; Harsha, Sree; Mlisana, Koleka

2016-01-01

The novel (1-(4-aryl)-1H-1,2,3-triazol-4-yl)methyl, substituted phenyl-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate derivatives were synthesized by the click reaction of the dihydropyrimidinones, bearing a terminal alkynyl group, with various substituted aryl azides at room temperature using a catalytic amount of Cu(OAc)2 and sodium ascorbate in a 1:2 ratio of acetone and water as a solvent. The newly synthesized compounds were characterized by a number of spectroscopic techniques, such as infrared, liquid chromatography-mass spectrometry, 1H, and 13C nuclear magnetic resonance along with single crystal X-ray diffraction. The current procedure for the synthesis of 1,2,3-triazole hybrids with dihydropyrimidinones is appropriate for the synthesis of a library of analogs 7a-l and the method accessible here is operationally simple and has excellent yields. The title compounds 7a-l were evaluated for their in vitro antitubercular activity against H37RV and multidrug-resistant strains of Mycobacterium tuberculosis by resazurin microplate assay plate method and it was found that compound 7d was promising against H37RV and multidrug-resistant strains of M. tuberculosis at 10 and 15 μg/mL, respectively. PMID:27601885

Design, synthesis, and characterization of (1-(4-aryl)- 1H-1,2,3-triazol-4-yl)methyl, substituted phenyl-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylates against Mycobacterium tuberculosis.

PubMed

Venugopala, Katharigatta N; Dharma Rao, G B; Bhandary, Subhrajyoti; Pillay, Melendhran; Chopra, Deepak; Aldhubiab, Bandar E; Attimarad, Mahesh; Alwassil, Osama Ibrahim; Harsha, Sree; Mlisana, Koleka

2016-01-01

The novel (1-(4-aryl)-1H-1,2,3-triazol-4-yl)methyl, substituted phenyl-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate derivatives were synthesized by the click reaction of the dihydropyrimidinones, bearing a terminal alkynyl group, with various substituted aryl azides at room temperature using a catalytic amount of Cu(OAc)2 and sodium ascorbate in a 1:2 ratio of acetone and water as a solvent. The newly synthesized compounds were characterized by a number of spectroscopic techniques, such as infrared, liquid chromatography-mass spectrometry, (1)H, and (13)C nuclear magnetic resonance along with single crystal X-ray diffraction. The current procedure for the synthesis of 1,2,3-triazole hybrids with dihydropyrimidinones is appropriate for the synthesis of a library of analogs 7a-l and the method accessible here is operationally simple and has excellent yields. The title compounds 7a-l were evaluated for their in vitro antitubercular activity against H37RV and multidrug-resistant strains of Mycobacterium tuberculosis by resazurin microplate assay plate method and it was found that compound 7d was promising against H37RV and multidrug-resistant strains of M. tuberculosis at 10 and 15 μg/mL, respectively.

Nanoscale modulations in (KLa)(CaW)O-6 and (NaLa)(CaW)O-6

DOE Office of Scientific and Technical Information (OSTI.GOV)

Licurse, Mark; Borisevich, Albina Y; Davies, Peter

2012-01-01

Complex nanoscale modulations are identified in two new A-site ordered perovskites, (KLa)(CaW)O{sub 6} and (NaLa)(CaW)O{sub 6}. In (KLa)(CaW)O{sub 6}, selected-area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM) show an incommensurate nanocheckerboard modulation with {approx}9.4 x 9.4 a{sub p} periodicity (a{sub p} {approx} 4 {angstrom} for the cubic perovskite aristotype). For (NaLa)(CaW)O{sub 6} a one-dimensional modulation is observed with a {approx}16(1 1 0)a{sub p} repeat; the <1 1 0> orientation of the nanostripes is different from the <1 0 0> stripes observed in other mixed A-site systems. Studies using high temperature x-ray diffraction suggest the formation of the complexmore » modulations is associated with small deviations from the ideal 1:1:1:1 stoichiometry of the (A{sup +}La{sup 3+})(CaW)O{sub 6} phases. Z-contrast images acquired on an aberration-corrected microscope provide evidence for deviations from stoichiometry with a {approx}1:15 periodic arrangement of La{sub 4/3}(CaW)O{sub 6}:(NaLa)(CaW)O{sub 6} nano-phases.« less

Syntheses, structures and magnetisms of copper(II)–azido coordination compounds with p-substituted benzoates as coligands

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Cuiyu; Yu, Nan; Bu, Huaitian

2016-01-15

Employing p-substituted benzoates with electron-withdrawing/electron-donating groups as coligands, four copper–azido compounds, [Cu{sub 1.5}(p-NO{sub 2}-benzoate)(N{sub 3}){sub 2}(H{sub 2}O)]{sub n} (1), [Cu(p-NO{sub 2}-benzoate)(N{sub 3})(H{sub 2}O)]{sub n} (2), [Cu(p-OH-benzoate)(N{sub 3})(H{sub 2}O)]{sub n}·nH{sub 2}O (3) and [Cu(p-CH{sub 3}-benzoate)(N{sub 3})]{sub n} (4), have been hydrothermally synthesized and structurally charactierized by single crystal X-ray diffraction. Structural analysis reveals that all compounds are composed of mixed EO-azido and syn–syn carboxylato-bridged Cu-N{sub 3}/COO chains. Compound 1 features the alternating triple-bridged (μ-EO-N{sub 3})(μ-COO)(μ-H{sub 2}O) and the double-bridged (EO-N{sub 3}){sub 2} modes. Both of 2 and 3 display the triple-bridged fashion (μ-EO-N{sub 3})(μ-COO)(μ-H{sub 2}O). While 4 exhibits the double-bridged modemore » (μ-EO-N{sub 3})(μ-COO). Based on hydrogen-bonding interactions, Cu–N{sub 3}/COO chains in 1–3 are further connected to form 3D supramolecular frameworks. As for compound 4, there are not hydrogen-bonding interactions when the p-CH{sub 3} substituted benzoate is employed as coligand. These compounds show intrachain ferromagnetic performance and different bulk properties. Remarkably, 1 features metamagnetism from antiferromagnetism to ferrimagnetism, while 3 reveals long-range ferromagnetic ordering between Cu(II) ions. Magneto-structural correlation has been also investigated. - Graphical abstract: With p-substituted benzoates as coligands, copper–azido compounds were isolated and structrually, magnetically characterized. Magneto-structural correlation has been investigated in detail.« less

Magnetic excitations and phonons simultaneously studied by resonant inelastic x-ray scattering in optimally doped Bi 1.5 Pb 0.55 Sr 1.6 La 0.4 CuO 6 + δ

DOE PAGES

Peng, Y. Y.; Hashimoto, M.; Sala, M. Moretti; ...

2015-08-24

In this paper, magnetic excitations in the optimally doped high-T c superconductor Bi 1.5Pb 0.55Sr 1.6La 0.4CuO 6+δ (OP-Bi2201, T c ≃ 34 K) are investigated by Cu L 3 edge resonant inelastic x-ray scattering (RIXS), below and above the pseudogap opening temperature. At both temperatures the broad spectral distribution disperses along the (1,0) direction up to ~350 meV at zone boundary, similar to other hole-doped cuprates. However, above ~0.22 reciprocal lattice units, we observe a concurrent intensity decrease for magnetic excitations and quasielastic signals with weak temperature dependence. This anomaly seems to indicate a coupling between magnetic, lattice, andmore » charge modes in this compound. We also compare the magnetic excitation spectra near the antinodal zone boundary in the single layer OP-Bi2201 and in the bilayer optimally doped Bi 1.5Pb 0.6Sr 1.54CaCu 2O 8+δ (OP-Bi2212, T c ≃ 96 K). Finally, the strong similarities in the paramagnon dispersion and in their energy at zone boundary indicate that the strength of the superexchange interaction and the short-range magnetic correlation cannot be directly related to T c, not even within the same family of cuprates.« less

Magnetic and magnetocaloric properties of La{sub 0.6}Pr{sub 0.1}Sr{sub 0.3}Mn{sub 1−x}Fe{sub x}O{sub 3} (0≤x≤0.3) manganites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cherif, R., E-mail: cherifrim18@yahoo.fr; Hlil, E.K.; Ellouze, M.

2014-07-01

The La{sub 0.6}Pr{sub 0.1}Sr{sub 0.3}Mn{sub 1−x}Fe{sub x}O{sub 3} (x=0, 0.1, 0.2 and 0.3) samples have been elaborated by the solid-state reaction method. X-ray powder diffraction shows that all the samples crystallize in a rhombohedric phase with R3{sup ¯}c space group. The variation of magnetization as a function of temperature and applied magnetic field was carried out. The samples for x=0 and 0.1 exhibit a FM–PM transition at the Curie temperature T{sub C}, however, for x=0.2 and 0.3 exhibit an AFM–PM one at the Neel temperature T{sub N}, when the temperature increases. A magneto-caloric effect has been calculated in terms ofmore » isothermal magnetic entropy change. A large magneto-caloric effect has been observed, the maximum entropy change, |ΔS{sub M}{sup max}|, reaches the highest value of 3.28 J/kgK under a magnetic field change of 5 T with an RCP value of 220 J/kg for La{sub 0.6}Pr{sub 0.1}Sr{sub 0.3}MnO{sub 3} composition, which will be an interesting compound for application materials working as magnetic refrigerants near room temperature. - Graphical abstract: Magnetic entropy change versus temperature and applied magnetic field for x=0.1 (a) and RCP versus applied magnetic field for x=0, 0.1 (b). - Highlights: • The La{sub 0.6}Pr{sub 0.1}Sr{sub 0.3}Mn{sub 1−x}Fe{sub x}O{sub 3} (0≤x≤0.3) polycrystalline samples were prepared by the solid state reaction method. • Crystalline and magnetic structures were investigated using DRX and magnetization measurements. • The magnetocaloric (MC) effect was estimated versus magnetic field and temperatures. • Compounds with x=0, 0.1 exhibit great potential for magnetic refrigeration at room temperature.« less

La{sup 3+} doping of the Sr{sub 2}CoWO{sub 6} double perovskite: A structural and magnetic study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lopez, C.A.; Viola, M.C.; Pedregosa, J.C.

2008-11-15

La-doped Sr{sub 2}CoWO{sub 6} double perovskites have been prepared in air in polycrystalline form by solid-state reaction. These materials have been studied by X-ray powder diffraction (XRPD), neutron powder diffraction (NPD) and magnetic susceptibility. The structural refinement was performed from combined XRPD and NPD data (D2B instrument, {lambda}=1.594 A). At room temperature, the replacement of Sr{sup 2+} by La{sup 3+} induces a change of the tetragonal structure, space group I4/m of the undoped Sr{sub 2}CoWO{sub 6} into the distorted monoclinic crystal structure, space group P2{sub 1}/n, Z=2. The structure of La-doped phases contains alternating CoO{sub 6} and (Co/W)O{sub 6} octahedra,more » almost fully ordered. On the other hand, the replacement of Sr{sup 2+} by La{sup 3+} induces a partial replacement of W{sup 6+} by Co{sup 2+} into the B sites, i.e. Sr{sub 2-x}La{sub x}CoW{sub 1-y}Co{sub y}O{sub 6} (y=x/4) with segregation of SrWO{sub 4}. Magnetic and neutron diffraction measurements indicate an antiferromagnetic ordering below T{sub N}=24 K independently of the La-substitution. - Graphical abstract: La-doped Sr{sub 2}CoWO{sub 6} double perovskites have been prepared in polycrystalline form by solid-state reaction. The general formula of these compounds is Sr{sub 2-x}La{sub x}CoW{sub 1-y}Co{sub y}O{sub 6} (y=x/4). XRPD, NPD and magnetic susceptibility studies were performed. The structure of monoclinic La-doped phases contains alternating CoO{sub 6} and (Co/W)O{sub 6} octahedra, almost fully ordered. NPD and magnetic measurements indicate an antiferromagnetic ordering at low temperature.« less

Nuclear blebbing of biologically active organoselenium compound towards human cervical cancer cell (HeLa): in vitro DNA/HSA binding, cleavage and cell imaging studies.

PubMed

Rizvi, Masood Ahmad; Zaki, Mehvash; Afzal, Mohd; Mane, Manoj; Kumar, Manjeet; Shah, Bhahwal Ali; Srivastav, Saurabh; Srikrishna, Saripella; Peerzada, Ghulam Mustafa; Tabassum, Sartaj

2015-01-27

New pharmacophore organoselenium compound (1) was designed, synthesized and characterized by various spectroscopic methods (IR, ESI-MS, (1)H, (13)C and (77)Se NMR) and further confirmed by X-ray crystallography. Compound 1 consists of two 3,5-bis(trifluoromethyl)phenyl units which are connected to the selenium atom via the organometallic C-Se bond. In vitro DNA binding studies of 1 was investigated by absorption and emission titration methods which revealed that 1 recognizes the minor groove of DNA in accordance with molecular docking studies with the DNA duplex. Gel electrophoretic assay demonstrates the ability of 1 to cleave pBR322 DNA through hydrolytic process which was further validated by T4 religation assay. To understand the drug-protein interaction of which ultimate molecular target was DNA, the affinity of 1 towards HSA was also investigated by the spectroscopic and molecular modeling techniques which showed hydrophobic interaction in the subdomain IIA of HSA. Furthermore, the intracellular localization of 1 was evidenced by cell imaging studies using HeLa cells. Copyright © 2014 Elsevier Masson SAS. All rights reserved.

Electronic band structure of LaCoO3/Y/Mn compounds

NASA Astrophysics Data System (ADS)

Rahnamaye Aliabad, H. A.; Hesam, V.; Ahmad, Iftikhar; Khan, Imad

2013-02-01

Spin polarization effects on electronic properties of pure LaCoO3 and doped compounds (La0.5Y0.5CoO3, LaCo0.5Mn0.5O3) in the rhombohedral phase have been studied. We have employed the full potential linearized augmented plane wave (FP-LAPW) method with the generalized gradient approximation (GGA+U) under density functional theory (DFT). The calculated band structures along with total as well as partial densities of states reveal that Y and Mn impurities have a significant effect on the structural and electronic properties of LaCoO3. It is found that Mn alters insulating behavior of this compound to the half metallic for spin up state. Obtained results show that the magnetic moment for the Co-3d state is near 3.12μB in LaCoO3 compound which increases and decreases with addition of Y and Mn dopants respectively.

Behavior of lanthanum containing barium stannate nanoparticles synthesized by cetyltriammonium bromide assisted wet chemistry route

NASA Astrophysics Data System (ADS)

Kumar, Astakala Anil; Kumar, Ashok; Quamara, J. K.

2018-02-01

In present study, we report dielectric, ferroelectric and pyroelectric behavior of pristine and La3+ containing barium stannate nanoparticles synthesized via wet chemical route involving cetyltriammonium bromide assisted thermal decomposition of binary precursors. The X-ray diffraction patterns of pristine and La3+ (2, 4 and 6 at%) doped BaSnO3 nanoparticles showed the formation of cubic perovskite phase. On substitution of Ba2+ lattice sites by La3+ at the La content of 6 at%, the sample exhibited fourfold increase in conductivity in comparison to pristine BaSnO3. Polarization hysteresis (P-E) curves of La containing barium stannate nanoparticles showed anti-ferroelectric behavior. The pyroelectric coefficient of pristine and La (2, 4 and 6 at%) containing BaSnO3 nanoparticles at 473 K were found to be 7.8, 11.6, 14.1 and 17.2 μCm-2K-1, respectively. Further, the responsivity and detectivity values were higher in comparison to the materials, such as AlN, GaN, CdS and ZnO.

Organic-Acid-Assisted Fabrication of Low-Cost Li-Rich Cathode Material (Li[Li1/6Fe1/6Ni1/6Mn1/2]O-2) for Lithium-Ion Battery

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Taolin; Chen, Shi; Li, Li

2014-12-24

A novel Li-rich cathode Li[Li1/6Fe1/6Ni1/6Mn1/2]O-2 (0.4Li(2)MnO(3-)0.6LiFe(1/3)Ni(1/3)Mn(1/3)O(2)) was synthesized by a solgel method, which uses citric acid (SC), tartaric acid (ST), or adipic acid (SA) as a chelating agent. The structural, morphological, and electrochemical properties of the prepared samples were characterized by various methods. X-ray diffraction showed that single-phase materials are formed mainly with typical alpha-NaFeO2 layered structure (R3 m), and the SC sample has the lowest Li/Ni cation disorder. The morphological study indicated homogeneous primary particles in good distribution size (100 nm) with small aggregates. The Fe, Ni, and Mn valences were determined by X-ray absorption near-edge structure analysis. Inmore » coin cell tests, the initial reversible discharge capacity of an SA electrode was 289.7 mAh g(-1) at the 0.1C rate in the 1.54.8 V voltage range, while an SC electrode showed a better cycling stability with relatively high capacity retention. At the 2C rate, the SC electrode can deliver a discharge capacity of 150 mAh g(-1) after 50 cycles. Differential capacity vs voltage curves were employed to further investigate the electrochemical reactions and the structural change process during cycling. This low-cost, Fe-based compound prepared by the solgel method has the potential to be used as the high capacity cathode material for Liion batteries.« less

Experimental and theoretical characterization of organic salt: 2-((4-bromophenyl)amino) pyrido[1,2-a] quinoxalin-11-ium bromide monohydrate synthesized via oxidative cyclization

NASA Astrophysics Data System (ADS)

Faizi, Md. Serajul Haque; Alam, Mohammad Jane; Haque, Ashanul; Ahmad, Shabbir; Shahid, M.; Ahmad, Musheer

2018-03-01

Quinoxalines are nitrogen-embedded heterocyclic compounds that possess unique and versatile pharmacological applications. The present article describes synthesis and characterization of organic salt 2-((4-bromophenyl)amino)pyrido [1,2-a]quinoxalin-11-ium bromide (BAPQ), an oxidative cyclized product of N-phenyl-N-(pyridine-2-ylmethylene)benzene-1,4-diamine (PPMD). The structure of the synthesized product was extensively characterized by 1H NMR, 2D-COSY NMR, MS, IR, UV-vis, X-ray techniques and elemental analysis. The electronic and structural properties of BAPQ was well complemented by performing extensive computational studies (B3LYP/6-311G (d,p) basis sets). Metal-free, mild reaction condition, easy work-up and excellent yield with high purity are main features of this work and thus holds promise for the generation of new compounds of this class. Analytical results indicated ionic nature of the compound with bromide as counterion. DFT calculation showed low kinetic stability and high reactivity of the compound.

Influence of Li3BO3 additives on the Li+ conductivity and stability of Ca/Ta-substituted Li6.55(La2.95Ca0.05)(Zr1.5Ta0.5)O12 electrolytes

NASA Astrophysics Data System (ADS)

Zhang, L. C.; Yang, J. F.; Gao, Y. X.; Wang, X. P.; Fang, Q. F.; Chen, C. H.

2017-07-01

The cubic Ca/Ta-substituted Li6.55(La2.95Ca0.05)(Zr1.5Ta0.5)O12 (LLCZTO) electrolytes were synthesized at 800 °C with Li3BO3 as additives. The optimal amount of Li3BO3 and its influences on the microstructure, crystal structures, Li+ conductivity and the stability of the Li6.55(La2.95Ca0.05)(Zr1.5Ta0.5)O12 were studied by SEM, XRD and EIS. Among all the samples, when the molar ratio of Li3BO3 to the Li6.55(La2.95Ca0.05)(Zr1.5Ta0.5)O12 is 4:5, the highest Li+ conductivity of 1.33 × 10-4 S cm-1 at 30 °C is obtained. When the LLCZTO samples are exposed in air, the Li+ conductivity is deteriorated possibly owing to the side reactions between the LLCZTO and the H2O or CO2 in the air. The Li3BO3 addition can alleviate such deterioration of the Li+ conductivity.

From {sub {infinity}}{sup 1}[(UO{sub 2}){sub 2}O(MoO{sub 4}){sub 4}]{sup 6-} to {sub {infinity}}{sup 1}[(UO{sub 2}){sub 2}(MoO{sub 4}){sub 3}(MoO{sub 5})]{sup 6-} infinite chains in A{sub 6}U{sub 2}Mo{sub 4}O{sub 21} (A=Na, K, Rb, Cs) compounds: Synthesis and crystal structure of Cs{sub 6}[(UO{sub 2}){sub 2}(MoO{sub 4}){sub 3}(MoO{sub 5})

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yagoubi, S.; Groupe de Radiochimie, Institut de Physique Nucleaire d'Orsay, Universite Paris-Sud XI, 91406 Orsay Cedex; Obbade, S., E-mail: said.obbade@phelma.grenoble-inp.f

2011-05-15

A new caesium uranyl molybdate belonging to the M{sub 6}U{sub 2}Mo{sub 4}O{sub 21} family has been synthesized by solid-state reaction and its structure determined from single-crystal X-ray diffraction data. Contrary to the other alkali uranyl molybdates of this family (A=Na, K, Rb) where molybdenum atoms adopt only tetrahedral coordination and which can be formulated A{sub 6}[(UO{sub 2}){sub 2}O(MoO{sub 4}){sub 4}], the caesium compound Cs{sub 6}U{sub 2}Mo{sub 4}O{sub 21} should be written Cs{sub 6}[(UO{sub 2}){sub 2}(MoO{sub 4}){sub 3}(MoO{sub 5})] with molybdenum atoms in tetrahedral and square pyramidal environments. Cs{sub 6}[(UO{sub 2}){sub 2}(MoO{sub 4}){sub 3}(MoO{sub 5})] crystallizes in the triclinic symmetry withmore » space group P1-bar and a=10.4275(14) A, b=15.075(2) A, c=17.806(2) A, {alpha}=70.72(1){sup o}, {beta}=80.38(1){sup o} and {gamma}=86.39(1){sup o}, V=2604.7(6) A{sup 3}, Z=4, {rho}{sub mes}=5.02(2) g/cm{sup 3} and {rho}{sub cal}=5.08(3) g/cm{sup 3}. A full-matrix least-squares refinement on the basis of F{sup 2} yielded R{sub 1}=0.0464 and wR{sub 2}=0.0950 for 596 parameters with 6964 independent reflections with I{>=}2{sigma}(I) collected on a BRUKER AXS diffractometer with Mo(K{alpha}) radiation and a CCD detector. The crystal structure of Cs compound is characterized by {sub {infinity}}{sup 1}[(UO{sub 2}){sub 2}(MoO{sub 4}){sub 3}(MoO{sub 5})]{sup 6-} parallels chains built from U{sub 2}O{sub 13} dimeric units, MoO{sub 4} tetrahedra and MoO{sub 5} square pyramids, whereas, Na, K and Rb compounds are characterized by {sub {infinity}}{sup 1}[(UO{sub 2}){sub 2}O(MoO{sub 4}){sub 4}]{sup 6-} parallel chains formulated simply of U{sub 2}O{sub 13} units and MoO{sub 4} tetrahedra. Infrared spectroscopy measurements using powdered samples synthesized by solid-state reaction, confirm the structural results. The thermal stability and the electrical conductivity are also studied. The four compounds decompose at low temperature (between 540 and 610

Une alternative au cobalt pour la synthese de nanotubes de carbone monoparoi par plasma inductif thermique

NASA Astrophysics Data System (ADS)

Carrier, Jean-Francois

Les nanotubes de carbone de type monoparoi (C-SWNT) sont une classe recente de nanomateriaux qui ont fait leur apparition en 1991. L'interet qu'on leur accorde provient des nombreuses proprietes d'avant-plan qu'ils possedent. Leur resistance mecanique serait des plus rigide, tout comme ils peuvent conduire l'electricite et la chaleur d'une maniere inegalee. Non moins, les C-SWNT promettent de devenir une nouvelle classe de plateforme moleculaire, en servant de site d'attache pour des groupements reactifs. Les promesses de ce type particulier de nanomateriau sont nombreuses, la question aujourd'hui est de comment les realiser. La technologie de synthese par plasma inductif thermique se situe avantageusement pour la qualite de ses produits, sa productivite et les faibles couts d'operation. Par contre, des recherches recentes ont permis de mettre en lumiere des risques d'expositions reliees a l'utilisation du cobalt, comme catalyseur de synthese; son elimination ou bien son remplacement est devenu une preoccupation importante. Quatre recettes alternatives ont ete mises a l'essai afin de trouver une alternative plus securitaire a la recette de base; un melange catalytique ternaire, compose de nickel, de cobalt et d'oxyde d'yttrium. La premiere consiste essentiellement a remplacer la proportion massique de cobalt par du nickel, qui etait deja present dans la recette de base. Les trois options suivantes contiennent de nouveaux catalyseurs, en remplacement au Co, qui sont apparus dans plusieurs recherches scientifiques au courant des dernieres annees: le dioxyde de zircone (ZrO2), dioxyde de manganese (MnO2) et le molybdene (Mo). La methode utilisee consiste a vaporiser la matiere premiere, sous forme solide, dans un reacteur plasma a haute frequence (3 MHz) a paroi refroidi. Apres le passage dans le plasma, le systeme traverse une section dite de "croissance", isolee thermiquement a l'aide de graphite, afin de maintenir une certaine plage de temperature favorable a la

Antioxidative and antiproliferative activities of novel pyrido[1,2-a]benzimidazoles.

PubMed

Tireli, Martina; Starčević, Kristina; Martinović, Tamara; Pavelić, Sandra Kraljević; Karminski-Zamola, Grace; Hranjec, Marijana

2017-02-01

A series of pyrido[1,2-a]benzimidazoles has been designed, and novel examples are synthesized and evaluated for their potential antiproliferative activity against four human tumour cell lines-cervical (HeLa), colorectal (SW620), breast (MCF-7) and hepatocellular carcinoma (HepG2). In addition, their antioxidative potency has been evaluated by in vitro spectrophotometric assays. Preliminary structure-activity relationships among the synthesized compounds are discussed. Evaluation of their antioxidative capacity has shown that two compounds (25 and 26) possess promising reducing characteristics and free radical scavenging activity. Selective antiproliferative effect in the single-digit micromolar range was observed for compound 25 on MCF-7 [Formula: see text] and HeLa [Formula: see text] cell lines, comparable to the standards 5-fluorouracil and cisplatin. The combination of the radical scavenging activity and antiproliferative activity of compound 25 positions this compound as a potential lead candidate for further optimization.

Unique (3,8)-connected lanthanide arenedisulfonate metal-organic frameworks containing benzimidazole-5,6-dicarboxylic acid co-ligand: Syntheses, structures and luminescence

NASA Astrophysics Data System (ADS)

Sun, Yan-Qiong; Liu, Qi; Zhong, Jie-Cen; Pan, Qun-Feng; Chen, Yi-Ping

2013-10-01

Two isostructural 3D lanthanide arenedisulfonate metal-organic frameworks (MOFs) [Ln(Hbidc)(nds)0.5(H2O)]n(Ln=Eu(1), La(2)) have been successfully synthesized by the hydrothermal reaction of lanthanide oxide with 2,6-naphthalenedisulfonate sodium (Na2nds) and an auxiliary ligand, 1H-benzimidazole-5,6-dicarboxylic acid (H3bidc). The two complexes are both constructed from 2D [Ln(Hbidc)]+ double layers pillared by nds2- ligands to generate 3D (3, 8)-connected open-framework structures with 1D long narrow channels running along the a axis. From topological point of view, the 3D framework is a (3, 8)-connected tfz-d net. The weak interactions including N-H⋯O, O-H⋯O hydrogen bonds and π-π stacking are observed in 1. The 2D IR correlation spectroscopy was applied to study the molecular interactions induced by thermal perturbation. The emission spectra of 1 exhibit the characteristic transition of 5D0→7FJ(J=0-4) of Eu(III).

Synthesizing new, high-temperature superconductors

NASA Astrophysics Data System (ADS)

Weaver, Claire; Aronson, Meigan

2015-03-01

Currently, there is no accepted theory behind type-II, high-temperature superconductors, but there is a distinct relationship between anti-ferromagnetism and superconductivity. Our research focuses on synthesizing new superconducting materials by observing the link between atomic structure and magnetic moments of anti-ferromagnetic compounds and attempting to reproduce the molecular physics of these known materials in new compounds. Consider the square-planar arrangement of the transition metal Fe in the Fe-pnictide superconductors of the ZrCuSiAs ``11 11'' and the ThCr2Si2 ``122'' structure types. We believe that the physics behind this superconductor, where Fe has d6 valence electrons, contributes to the superconducting state, not the presence of Fe itself. For this reason, we are synthesizing materials containing neighboring transition metals, like Mn and Co, combined with other elements in similar crystal lattice arrangements, having ionization properties that hopefully impose d6 valence electrons on the transition metals. This project was supported in part by the U.S. Department of Energy, Office of Science, Office of Workforce Development for Teachers and Scientists (WDTS) under the Science Undergraduate Laboratory Internships Program (SULI).

Synthesis and biological evaluation of substituted N-[3-(1H-pyrrol-1-yl)methyl]-1,2,5,6-tetrahydropyridin-1-yl]benzamide/benzene sulfonamides as anti-inflammatory agents.

PubMed

Gangapuram, Madhavi; Mazzio, Elizabeth; Eyunni, Suresh; Soliman, Karam F A; Redda, Kinfe K

2014-05-01

The pharmacological activities of tetrahydropyridine (THP) derivatives are dependent on the substituent ring moiety. In this study, we investigate the anti-inflammatory activities of 12 newly synthesized substituted N-[3-(1H-pyrrol-1-yl)methyl]-1,2,5,6-tetrahydrobenzamide/benzene sulfonamides (9a-l) in murine BV-2 microglial cells. All compounds were initially screened for attenuation of nitric oxide (NO) production in lipopolysaccharide (LPS) (1 µg/mL)-activated microglial cells. The data show that only SO2 -substituted THPs were effective at sub-lethal concentrations (IC50 values of 12.92 µM (9i), 14.64 µM (9j), 19.63 µM (9k)) relative to L-N6-(1-iminoethyl)lysine positive control (IC50  = 3.1 µM). The most potent SO2 -substituted compound (9i) also blocked the LPS-inducible nitric oxide synthase (iNOS) and attenuated the release of several cytokines including IL-1α, IL-10, and IL-6. These findings establish the moderate immuno-modulating effects of SO2 -substituted THP derivatives. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Experimental and theoretical studies on tautomeric structures of a newly synthesized 2,2‧(hydrazine-1,2-diylidenebis(propan-1-yl-1-ylidene))diphenol

NASA Astrophysics Data System (ADS)

Karakurt, Tuncay; Cukurovali, Alaaddin; Subasi, Nuriye Tuna; Onaran, Abdurrahman; Ece, Abdulilah; Eker, Sıtkı; Kani, Ibrahim

2018-02-01

In the present study, a single crystal of a Schiff base, 2,2‧(hydrazine-1,2-diylidenebis(propan-1-yl-1-ylidene))diphenol, was synthesized. The structure of the synthesized crystal was confirmed by 1H and 13C NMR spectroscopic and X-ray diffraction analysis techniques. Experimental and theoretical studies were carried out on two tautomeric structures. It has been observed that the title compound studied can be in two different tautomeric forms, phenol-imine and keto-amine. Theoretical calculations have been performed to support experimental results. Accordingly, the geometric parameters of the compound were optimized by the density functional theory (DFT) method using the Gaussian 09 and Quantum Espresso (QE) packet program was used for periodic boundary conditions (PBC) studies. Furthermore, the compound was also tested for in vitro antifungal activity against Sclerotinia sclerotiorum, Alternaria solani, Fusarium oxysporum f. sp. lycopersici and Monilinia fructigena plant pathogens. Promising inhibition profiles were observed especially towards A. solani. Finally, molecular docking studies and post-docking procedure based on Molecular Mechanics-Generalized Born Surface Area (MM-GBSA) were also carried out to get insight into the compound's binding interactions with the potential. Although theoretical calculations showed that the phenol-imine form was more stable, keto-amine form was predicted to have better binding affinity which was concluded to result from loss of rotational entropy in phenol-imine upon binding. The results obtained here from both experimental and computational methods might serve as a potential lead in the development of novel anti-fungal agents.

Isolation, purification, and characterization of antimicrobial compound 6-[1,2-dimethyl-6-(2-methyl-allyloxy)-hexyl]-3-(2-methoxy-phenyl)-chromen-4-one from Penicillium sp. HT-28.

PubMed

Kaur, Harpreet; Arora, Daljit Singh; Sharma, Vishal

2014-08-01

A fungal culture (Penicillium sp., HT-28), isolated from soil has been evaluated for its bioactivity, which showed broad spectrum antimicrobial activity and was effective against methicillin-resistant Staphylococcus aureus (MRSA) also. Statistical optimization of the medium by response surface methodology (RSM) enhanced the antimicrobial activity up to 1.8-fold. Column chromatography was used to isolate the active compound (A), which was characterized to be 6-[1,2-dimethyl-6-(2-methyl-allyloxy)-hexyl]-3-(2-methoxy-phenyl)-chromen-4-one by various spectroscopic techniques such as infrared (IR), (1)H and (13)C nuclear magnetic resonance (NMR) spectra, and mass spectroscopy. Minimum inhibitory concentration (MIC) of the active compound (A) ranged from 0.5 to 15 μg/mL. Viable cell count studies of the active compound (A) showed S. aureus, Escherichia coli, Staphylococcus epidermidis, and Salmonella typhimurium 1 to be the most sensitive. The compound retained its bioactivity after treating it at 100 °C for 1 h. Furthermore, the compound (A) when tested for its biosafety was found neither to be cytotoxic nor mutagenic. The study demonstrated that an apparently novel compound isolated from Penicillium sp. (HT-28) seems to be a stable and potent antimicrobial.

Synthesis, structure characterization and biological studies on a new aromatic hydrazone, 5-(2-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)hydrazono)-2,2-dimethyl-1,3-dioxane-4,6-dione, and its transition metal complexes

NASA Astrophysics Data System (ADS)

Kumar, Shubha S.; Biju, S.; Sadasivan, V.

2018-03-01

A new aromatic hydrazone 5-(2-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)hydrazono)-2,2-dimethyl-1,3-dioxane-4,6-dione has been synthesized by Japp-Klingemann reaction from diazotized 4-aminoantipyrine and Meldrum's acid. A few 3d-metal ion complexes of this hydrazone were synthesized. The compound and its complexes were characterized by UV-Visible, 1H NMR, ESR, Mass spectral, molar conductance and magnetic susceptibility measurements. The compound was found to exist in hydrazone form in solid state and solution from SXRD and 1H NMR study. The influence of pH on the molecule was studied and found that it shows azo/enol-hydrazone tautomerism in solution. This molecule act as a univalent tridentate ligand and the complexes were assigned to have a 1:2 stoichiometry (M:L). The antioxidant properties of the compounds were explored by DPPH assay and found that the ligand possesses better free radical scavenging effect than the complexes. Antimicrobial activities of these compounds were investigated and were found to be active.

Synthesis and anti-HIV activity of novel 3-substituted phenyl-6,7-dimethoxy-3a,4-dihydro-3H-indeno[1,2-c]isoxazole analogues.

PubMed

Ali, Mohamed A; Ismail, Rusli; Choon, Tan S; Yoon, Yeong K; Wei, Ang C; Pandian, Suresh; Samy, Jeyabalan G; De Clercq, Eric; Pannecouque, Christophe

2011-01-01

A series of novel 3-(substituted phenyl)-6,7-dimethoxy-3a,4-dihydro-3H-indeno[1,2-c]isoxazole analogues were synthesized by the reaction of 5,6-dimethoxy-2-[(E)-1-phenylmethylidene]-1-indanone with hydroxylamine hydrochloride. The title compounds were tested for their in vitro anti-HIV activity. Among the compounds, (4g) showed a promising anti-HIV activity in the in vitro testing against IIIB and ROD strains. The IC50 of both IIIB and ROD were found to be 9.05 microM and > 125 microM, respectively.

Deuteration and fluorination of 1,3-bis(2-phenylethyl)pyrimidine-2,4,6(1H,3H,5H)-trione to improve its pharmacokinetic properties.

PubMed

Xia, Guoyao; Benmohamed, Radhia; Morimoto, Richard I; Kirsch, Donald R; Silverman, Richard B

2014-11-01

Amyotrophic lateral sclerosis (ALS) is a fatal neurodegenerative disease characterized by the progressive loss of motor neurons, leading to muscle weakness, paralysis, and death, most often from respiratory failure. Over 200 pyrimidine-2,4,6-trione (PYT) small molecules, which prevent aggregation and reduce the associated toxicity of mutant superoxide dismutase 1 (SOD1) found in patients with familial ALS, have been synthesized and tested. One of the compounds (1,3-bis(2-phenylethyl)pyrimidine-2,4,6(1H,3H,5H)-trione, (1) was previously found to have an excellent combination of potency efficacy, and some desirable pharmacokinetic properties. To improve the solubility and metabolic stability properties of this compound, deuterium and fluorine were introduced into 1. New analogs with better solubility, plasma stability, and human microsome stability were identified. Copyright © 2014 Elsevier Ltd. All rights reserved.

Identification, Synthesis, and Biological Evaluation of the Metabolites of 3-Amino-6-(3'-aminopropyl)-5H-indeno[1,2-c]isoquinoline-5,11-(6H)dione (AM6-36), a Promising Rexinoid Lead Compound for the Development of Cancer Chemotherapeutic and Chemopreventive Agents

PubMed Central

Chen, Lian; Conda-Sheridan, Martin; Narasimha Reddy, P. V.; Morrell, Andrew; Park, Eun-Jung; Kondratyuk, Tamara P.; Pezzuto, John M.; van Breemen, Richard B.; Cushman, Mark

2012-01-01

Activation of the retinoid X receptor (RXR), which is involved in cell proliferation, differentiation and apoptosis, is a strategy for cancer chemotherapy and chemoprevention, and 3-amino-6-(3'-aminopropyl)-5H-indeno[1,2-c]isoquinoline-5,11-(6H)dione (AM6-36) (3) is among the few RXR ligands known. The presently reported studies of 3 include its binding to human plasma proteins, metabolic stability using human liver microsomes, metabolism by human liver microsomes and hepatocytes, and in vivo disposition in rat serum, liver and mammary tissue. Compound 3 was 75% bound to human plasma proteins, and its metabolic stability was much greater than propranolol. One phase I metabolite was formed by human liver microsomes, 7 phase I and II metabolites were formed by human hepatocytes, and 5 metabolites were detected in rat serum and liver after oral administration. The putative metabolites predicted using LC-MS-MS were synthesized to confirm their structures and to provide sufficient material for investigation of induction of RXRE transcriptional activity and inhibition of NFκB. PMID:22712432

Identification, synthesis, and biological evaluation of the metabolites of 3-amino-6-(3'-aminopropyl)-5H-indeno[1,2-c]isoquinoline-5,11-(6H)dione (AM6-36), a promising rexinoid lead compound for the development of cancer chemotherapeutic and chemopreventive agents.

PubMed

Chen, Lian; Conda-Sheridan, Martin; Reddy, P V Narasimha; Morrell, Andrew; Park, Eun-Jung; Kondratyuk, Tamara P; Pezzuto, John M; van Breemen, Richard B; Cushman, Mark

2012-06-28

Activation of the retinoid X receptor (RXR), which is involved in cell proliferation, differentiation, and apoptosis, is a strategy for cancer chemotherapy and chemoprevention, and 3-amino-6-(3'-aminopropyl)-5H-indeno[1,2-c]isoquinoline-5,11-(6H)dione (AM6-36) (3) is among the few RXR ligands known. The presently reported studies of 3 include its binding to human plasma proteins, metabolic stability using human liver microsomes, metabolism by human liver microsomes and hepatocytes, and in vivo disposition in rat serum, liver, and mammary tissue. Compound 3 was 75% bound to human plasma proteins, and its metabolic stability was much greater than propranolol. One phase I metabolite was formed by human liver microsomes, seven phase I and II metabolites were formed by human hepatocytes, and five metabolites were detected in rat serum and liver after oral administration. The putative metabolites predicted using LC-MS-MS were synthesized to confirm their structures and to provide sufficient material for investigation of induction of RXRE transcriptional activity and inhibition of NFκB.

Structural diversity of four coordination polymers based on 5-nitro-1,2,3-benzenetricarboxylic acid (H3nbta): Solvothermal syntheses, structural characterizations and properties

NASA Astrophysics Data System (ADS)

Shi, Chenjie; Wang, Zikai; Chen, Yifan; Zhang, Xiaoyu; Zhao, Yue; Tao, Yuehong; Wu, Hua

2017-09-01

Four 3D coordination compounds, named [Cd3(nbta)2(bix)2(H2O)2]·H2O (1), Zn3(nbta)2(biim)3 (2), Zn6(nbta)4(btd)5 (3) and [Co3(nbta)2(bid)(H2O)8]·4H2O (4) (bix=1,4-bis(imidazole-1-ylmethyl)benzene, biim=1,1‧-(1,4-butanediyl)bis(imidazole), btd=1,10-bis(1,2,4-triazol-1-yl)decane, bid=1,10-bis(imidazole-1-yl)decane), and H3nbta=5-nitro-1,2,3-benzenetricarboxylic acid), have been synthesized by solvothermal methods and structurally characterized by X-ray diffraction studies. In compound 1, every nbta3- anion connects four CdII ions to give a 2D layer, and the layers are pillared by bix ligands to generate a 3D framework with a Schläfli symbol of (3·4·63·7)(4·64·8)(43·63)(34·42·66·76·88·92). For compound 2, every nbta3- anion connects three ZnII ions to give a 2D layer structure, the 2D layers are further connected into a facinating 3D framework by biim ligands with (3,4)-connected (3·6·7)(3·5·62·7·8)(3·52·6·8·9)(5·6·8·10·112) topology. In compound 3, the nbta3- anions are connected by ZnII ions to generate a 2D layer, and the layers are bridged by btd ligands to build a fascinating 3D framework with (4·6·7·8·92)(4·6·8·92·10)(4·93·102)(4·6·8·9·102)(4·6·7·8·9·10)(4·6·7·8·102)(42·6·7·8·9) topology. In compound 4, the nbta3- aions are connected by CoII ions into a 2D layer, the 2D layers are linked by bid ligands to generate a 3D 103 topological framework. Furthermore, the IR spectra, TGA, PXRD, elemental analyses, the solid-state luminescence of compounds 1-3 have been studied.

Catalytic pyrolysis of model compounds and waste cooking oil for production of light olefins over La/ZSM-5 catalysts

NASA Astrophysics Data System (ADS)

Li, F. W.; Ding, S. L.; Li, L.; Gao, C.; Zhong, Z.; Wang, S. X.; Li, Z. X.

2016-08-01

Waste cooking oil (WCO) and its model compounds (oleic acid and methyl laurate) are catalytically pyrolyzed in a fixed-bed reactor over La modified ZSM-5 catalysts (La/ZSM-5) aiming for production of C2-C4 light olefins. The LaO content in catalysts was set at 0, 2, 6, 10 and 14 wt%. The gas and liquid products are analyzed. The La/ZSM-5 catalyst with 6% LaO showed higher selectivity to light olefins when WCO and methyl laurate were pyrolyzed, and olefin content was 26% for WCO and 21% for methyl laurate. The catalyst with 10% LaO showed high selectivity to light olefins (28.5%) when oleic acid was pyrolyzed. The liquid products from WCO and model compounds mainly contain esters and aromatic hydrocarbons. More esters were observed in liquid products from methyl laurate and WCO pyrolysis, indicating that it is more difficult to pyrolyze esters and WCO than oleic acid. The coked catalysts were analyzed by temperature-programmed oxidation. The result shows that graphite is the main component of coke. The conversion of WCO to light olefins potentially provides an alternative and sustainable route for production of the key petrochemicals.

Novel microtubule-targeted agent 6-chloro-4-(methoxyphenyl) coumarin induces G2-M arrest and apoptosis in HeLa cells

PubMed Central

Ma, Yi-ming; Zhou, Yu-bo; Xie, Chuan-ming; Chen, Dong-mei; Li, Jia

2012-01-01

Aim: To identify a novel coumarin analogue with the highest anticancer activity and to further investigate its anticancer mechanisms. Methods: The viability of cancer cells was investigated using the MTT assay. The cell cycle progression was evaluated using both flow cytometric and Western blotting analysis. Microtubule depolymerization was observed with immunocytochemistry in vivo and a tubulin depolymerization assay in vitro. Apoptosis was demonstrated using Annexin V/Propidium Iodide (PI) double-staining and sub-G1 analysis. Results: Among 36 analogues of coumarin, 6-chloro-4-(methoxyphenyl) coumarin showed the best anticancer activity (IC50 value about 200 nmol/L) in HCT116 cells. The compound had a broad spectrum of anticancer activity against 9 cancer cell lines derived from colon cancer, breast cancer, liver cancer, cervical cancer, leukemia, epidermoid cancer with IC50 value of 75 nmol/L–1.57 μmol/L but with low cytotocitity against WI-38 human lung fibroblasts (IC50 value of 12.128 μmol/L). The compound (0.04–10 μmol/L) induced G2-M phase arrest in HeLa cells in a dose-dependent manner, which was reversible after the compound was removed. The compound (10–300 μmol/L) induced the depolymerization of purified porcine tubulin in vitro. Finally, the compound (0.04–2.5 μmol/L) induced apoptosis of HeLa cells in dose- and time-dependent manners. Conclusion: 6-Chloro-4-(methoxyphenyl) coumarin is a novel microtubule-targeting agent that induces G2–M arrest and apoptosis in HeLa cells. PMID:22266726

Fused heterocyclic compounds bearing bridgehead nitrogen as potent HIV-1 NNRTIs. Part 1: design, synthesis and biological evaluation of novel 5,7-disubstituted pyrazolo[1,5-a]pyrimidine derivatives.

PubMed

Tian, Ye; Du, Deping; Rai, Diwakar; Wang, Liu; Liu, Huiqing; Zhan, Peng; De Clercq, Erik; Pannecouque, Christophe; Liu, Xinyong

2014-04-01

In our continuous efforts to identify novel potent HIV-1 NNRTIs, a novel class of 5,7-disubstituted pyrazolo[1,5-a]pyrimidine derivatives were rationally designed, synthesized and evaluated for their anti-HIV activities in MT4 cell cultures. Biological results showed that most of the tested compounds displayed excellent activity against wild-type HIV-1 with a wide range of EC50 values from 5.98 to 0.07μM. Among the active compounds, 5a was found to be the most promising analogue with an EC50 of 0.07μM against wild-type HIV-1 and very high selectivity index (SI, 3999). Compound 5a was more effective than the reference drugs nevirapine (by 2-fold) and delavirdine (by 2-fold). In order to further confirm their binding target, an HIV-1 RT inhibitory assay was also performed. Furthermore, SAR analysis among the newly synthesized compounds was discussed and the binding mode of the active compound 5a was rationalized by molecular modeling studies. Copyright © 2014 Elsevier Ltd. All rights reserved.

Carbon chemistry: The high temperature syntheses and applications of nanotubes andsp-hybridized compounds

NASA Astrophysics Data System (ADS)

Mitchell, Daniel Robert

A brief introduction to carbon chemistry is given with an emphasis on the use high-temperature reactions that use carbon vapor, generated from graphite, to synthesize nano-structured materials. Laser and electric are ablation of graphite was utilized to create a variety of high carbon content materials ranging from discrete acetylenic molecules to extremely large multi-wall nanotubes. A new synthesis for large carbon nanotubes, containing 1--5 atom percent nitrogen bound into the graphite lattice, was realized by the reaction of carbon vapor, nickel/yttrium catalyst and cyanogen gas. These carbon "megatubes" were then employed as a substrate to tether a wide variety of molecules both inorganic and organic. The megatubes, in their native and derivatized states, were then assembled into simple circuits to explore their electronic transport properties. Direct fluorination was used to post-treat the surface of the multi-wall carbon nanotubes in order to alter the inherent physical and chemical properties of the tubes, as well as to serve as another route to functionalize their surfaces. Fluorine sites on the walls of the tube were allowed to react with Grignard reagents to produce nantoubes with the chosen alkyl chemically bonded to the surface. Products were characterized with techniques similar to unfluorinated tubules. Using similar carbon vaporization techniques, sp-hybridized carbon chain compounds were synthesized. Using a one-step method dicyanopolyynes were synthesized and characterized with nuclear magnetic resonance and mass spectroscopy, containing up to 8 acetylenic repeat units. A two-step method was also utilized to create polyynes terminated with trifluoromethyl or nitrile radicals generated in a capacitively coupled radio frequency glow plasma discharge. A partial characterization of these products was accomplished with nuclear magnetic resonance, mass, and infrared spectroscopy techniques.

Synthesis, Characterization, and Biological Evaluation of certain 6-methyl-2(3H)-benzo-1, 3-thiazolyl-1'-ethylidene-2-(o, p- Substituted Acetophenones) Hydrazine Analogs.

PubMed

Alang, G; Kaur, G; Kaur, R; Singh, A; Tiwari, R

2010-10-01

In the present study, five new derivatives (GG4 to GG8) of benzothiazoles were synthesized and evaluated against Staphylococcus aureus (MTCC 737), Pseudomonas aeruginosa (MTCC 424), Escherichia coli (MTCC 1687), and yeast-like fungi Candida tropicalis. p-Toluidine on treatment with ammonium thiocynate formed 2-benzothiazolamines (II), which on reaction with hydrazine hydrate formed a hydrazino derivative (III). Compounds GG4 to GG8 were synthesized by reacting the hydrazine derivative with different acetophenones. All the synthesized compounds were identified by IR and (1)H-NMR, and antimicrobial activity was performed on the synthesized compounds. Presence of NO(2), Br, OCH(3), and Cl groups to the substituted benzothiazole enhanced the antibacterial and antifungal activities.

Preparation of LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphors by a facile precursor method and their luminescent properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Xia; Liang, Pan; Huang, Hong-Sheng

2014-04-01

Graphical abstract: LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor was obtained by calcining the precursor which was synthesized by boric acid melting method. It (a) exhibits much stronger PL intensity than that (b) prepared by conventional solid state reaction method. - Highlights: • A calcining precursor method was used for preparation of LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor. • Precursor was prepared by boric acid melting method. • The luminescence intensity of LaB{sub 3}O{sub 6}:Eu{sup 3+} was enhanced by the present method. - Abstract: The LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphors were prepared by calcining the precursors which were synthesized by boric acid meltingmore » method using rare earth oxide and boric acid as raw materials, and they were characterized by EDS, XRD, IR, SEM and PL. The influences of reaction temperature for the preparation of precursor and subsequent calcination temperature and time of precursor on the luminescence properties of LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor were investigated. The results showed that the LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphors with maximum luminescent intensity were obtained by calcining precursor at 1000 °C for 6 h, in which the precursor was prepared at 200 °C for 72 h. Compared with the conventional high temperature solid-state reaction method, the pure LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor can be obtained at relatively lower calcination temperature by the precursor method and exhibits much stronger emission intensity.« less

Two-dimensional 3d-4f heterometallic coordination polymers: syntheses, crystal structures, and magnetic properties of six new Co(II)-Ln(III) compounds.

PubMed

Díaz-Gallifa, Pau; Fabelo, Oscar; Pasán, Jorge; Cañadillas-Delgado, Laura; Lloret, Francesc; Julve, Miguel; Ruiz-Pérez, Catalina

2014-06-16

Six new heterometallic cobalt(II)-lanthanide(III) complexes of formulas [Ln(bta)(H2O)2]2[Co(H2O)6]·10H2O [Ln = Nd(III) (1) and Eu(III) (2)] and [Ln2Co(bta)2(H2O)8]n·6nH2O [Ln = Eu(III) (3), Sm(III) (4), Gd(III) (5), and Tb(III) (6)] (H4bta = 1,2,4,5-benzenetretracaboxylic acid) have been synthesized and characterized via single-crystal X-ray diffraction. 1 and 2 are isostructural compounds with a structure composed of anionic layers of [Ln(bta)(H2O)2]n(n-) sandwiching mononuclear [Co(H2O)6](2+) cations plus crystallization water molecules, which are interlinked by electrostatic forces and hydrogen bonds, leading to a supramolecular three-dimensional network. 3-6 are also isostructural compounds, and their structure consists of neutral layers of formula [Ln2Co(bta)2(H2O)8]n and crystallization water molecules, which are connected through hydrogen bonds to afford a supramolecular three-dimensional network. Heterometallic chains formed by the regular alternation of two nine-coordinate lanthanide(III) polyhedra [Ln(III)O9] and one compressed cobalt(II) octahedron [Co(II)O6] along the crystallographic c-axis are cross-linked by bta ligands within each layer of 3-6. Magnetic susceptibility measurements on polycrystalline samples for 3-6 have been carried out in the temperature range of 2.0-300 K. The magnetic behavior of these types of Ln(III)-Co(II) complexes, which have been modeled by using matrix dagonalization techniques, reveals the lack of magnetic coupling for 3 and 4, and the occurrence of weak antiferromagnetic interactions within the Gd(III)-Gd(III) (5) and Tb(III)-Tb(III) (6) dinuclear units through the exchange pathway provided by the double oxo(carboxylate) and double syn-syn carboxylate bridges.

Two Types of 2D Layered Iodoargentates Based on Trimeric [Ag3I7] Secondary Building Units and Hexameric [Ag6I12] Ternary Building Units: Syntheses, Crystal Structures, and Efficient Visible Light Responding Photocatalytic Properties.

PubMed

Lei, Xiao-Wu; Yue, Cheng-Yang; Zhao, Jian-Qiang; Han, Yong-Fang; Yang, Jiang-Tao; Meng, Rong-Rong; Gao, Chuan-Sheng; Ding, Hao; Wang, Chun-Yan; Chen, Wan-Dong; Hong, Mao-Chun

2015-11-16

With mixed transition-metal-complex, alkali-metal, or organic cations as structure-directing agents, a series of novel two-dimensional (2D) layered inorganic-organic hybrid iodoargentates, namely, Kx[TM(2,2-bipy)3]2Ag6I11 (TM = Mn (1), Fe (2), Co (3), Ni (4), Zn (5); x = 0.89-1) and [(Ni(2,2-bipy)3][H-2,2-bipy]Ag3I6 (6), have been solvothermally synthesized and structurally characterized. All the title compounds feature 2D microporous layers composed by [Ag3I7] secondary building units based on AgI4 tetrahedra. Differently, the [Ag3I7] trimers are directly interconnected via corner-sharing to form the 2D [Ag6I11](5-) layer in compounds 1-5, whereas two neighboring [Ag3I7] trimers are initially condensed into a hexameric [Ag6I12] ternary building unit as a new node, which further self-assembles, leading to the 2D [Ag6I10](4-) layer in compound 6. The UV-vis diffuse-reflectance measurements reveal that all the compounds possess proper semiconductor behaviors with tunable band gaps of 1.66-2.75 eV, which lead to highly efficient photocatalytic degradation activities over organic pollutants under visible light irradiation compared to that of N-dotted P25. Interestingly, all the samples feature distinct photodegradative speeds at the same reaction conditions, and compound 1 features the highest photocatalytic activity among the title phases. The luminescence properties, band structures, and thermal stabilities were also studied.

Synthesis and structure determination of the novel aluminophosphate TL-1: A new layered compound with corner-sharing AlX{sub 6} chains

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pastero, Linda; Interdepartmental Centre “Nanostructured Interfaces and Surfaces-NIS”, Via Quarello 15A, 10135 Torino; CrisDi – Interdepartmental Center for Crystallography, Università di Torino, Via Pietro Giuria 7, I-10125 Torino

2016-10-15

A novel layered aluminophosphate (TL-1) has been synthesized. Crystals grow as pseudo-hexagonal thin platelets and their whole morphology depends on the synthesis conditions. The structure was solved by single-crystal X-ray diffraction using charge flipping methods. The synthesized layered material, with composition [AlPO{sub 4}F(H{sub 2}O)]-(H{sub 10}C{sub 4}ON){sub 4}, crystallizes in the monoclinic space group P2{sub 1}/a with a=9.2282(5) Å, b=6.9152(4) Å, c=14.4615(9) Å, β=101.57(1)°. The novel compound has corner sharing AlO{sub 3}F{sub 2}(H{sub 2}O) octahedral chains running along [010], where fluorine atoms are at the shared apices, three oxygen atoms are shared with PO{sub 4} tetrahedra while the sixth oxygen pertainmore » to an H{sub 2}O molecule. The stability field of the novel material is enclosed in the HF/Al{sub 2}O{sub 3} ratio ranging between 1 and 4 and the HF/morpholine ratio lower than 3. At temperature lower than 190 °C, the synthesis results is a pure aluminophosphate sample (low alumina/morpholine ratio). A treatment with H{sub 2}CO{sub 3} leads to a complete morpholine removal, as shown by in situ Raman spectroscopy. Powder X-ray diffraction reveals that, after morpholine extraction, the material collapses. The collapse is irreversible. - Highlights: • A new layered aluminophosphate was obtained and characterized. • The crystal structure is a sequence of aluminophosphate and organic layers. • The stability field of the new phase was defined by changing chemistry and T. • The templating agent can be removed by using a CO{sub 2} aqueous solution. • The decomposition of the morpholine induce a collapse in the structure.« less

Telluride Misfit Layer Compounds: [(PbTe) 1.17 ] m (TiTe 2 ) n

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moore, Daniel B.; Beekman, Matt; Disch, Sabrina

Telluride misfit layer compounds are reported for the first time. These compounds were synthesized using a novel approach of structurally designing a precursor that would form the desired product upon low-temperature annealing, which allows the synthesis of kinetically stable products that do not appear on the equilibrium phase diagram. Four new compounds of the [(PbTe)1.17]m(TiTe2)n family are reported, and their structures were examined by a variety of X-ray diffraction techniques.

Telluride Misfit Layer Compounds: [(PbTe) 1.17 ] m (TiTe 2 ) n

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moore, Daniel B.; Beekman, Matt; Disch, Sabrina

2014-04-09

Telluride misfit layer compounds are reported for the first time. These compounds were synthesized using a novel approach of structurally designing a precursor that would form the desired product upon low-temperature annealing, which allows the synthesis of kinetically stable products that do not appear on the equilibrium phase diagram. Four new compounds of the [(PbTe)1.17]m(TiTe2)n family are reported, and their structures were examined by a variety of X-ray diffraction techniques.

Synthesis, Characterization, and Biological Evaluation of certain 6-methyl-2(3H)-benzo-1, 3-thiazolyl-1’-ethylidene-2-(o, p- Substituted Acetophenones) Hydrazine Analogs

PubMed Central

Alang, G; Kaur, G; Kaur, R; Singh, A; Tiwari, R

2010-01-01

In the present study, five new derivatives (GG4 to GG8) of benzothiazoles were synthesized and evaluated against Staphylococcus aureus (MTCC 737), Pseudomonas aeruginosa (MTCC 424), Escherichia coli (MTCC 1687), and yeast-like fungi Candida tropicalis. p-Toluidine on treatment with ammonium thiocynate formed 2-benzothiazolamines (II), which on reaction with hydrazine hydrate formed a hydrazino derivative (III). Compounds GG4 to GG8 were synthesized by reacting the hydrazine derivative with different acetophenones. All the synthesized compounds were identified by IR and 1H-NMR, and antimicrobial activity was performed on the synthesized compounds. Presence of NO2, Br, OCH3, and Cl groups to the substituted benzothiazole enhanced the antibacterial and antifungal activities. PMID:21264101

Corrosion inhibition of mild steel in 1M HCl by D-glucose derivatives of dihydropyrido [2,3-d:6,5-d′] dipyrimidine-2, 4, 6, 8(1H,3H, 5H,7H)-tetraone

PubMed Central

Verma, Chandrabhan; Quraishi, M. A.; Kluza, K.; Makowska-Janusik, M.; Olasunkanmi, Lukman O.; Ebenso, Eno E.

2017-01-01

D-glucose derivatives of dihydropyrido-[2,3-d:6,5-d′]-dipyrimidine-2, 4, 6, 8(1H,3H, 5H,7H)-tetraone (GPHs) have been synthesized and investigated as corrosion inhibitors for mild steel in 1M HCl solution using gravimetric, electrochemical, surface, quantum chemical calculations and Monte Carlo simulations methods. The order of inhibition efficiencies is GPH-3 > GPH-2 > GPH-1. The results further showed that the inhibitor molecules with electron releasing (-OH, -OCH3) substituents exhibit higher efficiency than the parent molecule without any substituents. Polarization study suggests that the studied compounds are mixed-type but exhibited predominantly cathodic inhibitive effect. The adsorption of these compounds on mild steel surface obeyed the Langmuir adsorption isotherm. SEM, EDX and AFM analyses were used to confirm the inhibitive actions of the molecules on mild steel surface. Quantum chemical (QC) calculations and Monte Carlo (MC) simulations studies were undertaken to further corroborate the experimental results. PMID:28317849

Interplay of 3 d - and 5 d -sublattice magnetism in the double perovskite substitution series La2Zn1 -xCoxIrO6

NASA Astrophysics Data System (ADS)

Vogl, M.; Corredor, L. T.; Dey, T.; Morrow, R.; Scaravaggi, F.; Wolter, A. U. B.; Aswartham, S.; Wurmehl, S.; Büchner, B.

2018-01-01

We report on the interplay of 3 d - and 5 d -sublattice magnetism in polycrystalline samples of the double perovskite substitution series La2Zn1 -xCoxIrO6 . Powder x-ray diffraction reveals no major structural changes within the series. In magnetization measurements, a gradual shift of the transition temperature from TN ≈91 K for the Co parent compound to TN ≈8.7 K for the Zn parent compound is observed. The data on the Zn-rich members of the substitution series indicate that this is accompanied by changing roles of the 3 d sublattice of Co2 + and the strongly spin-orbit coupled 5 d -sublattice of Ir4 + with its jeff=1 /2 ground state, as a function of the Co/Zn ratio. Temperature-dependent specific-heat studies revealed a reduced magnetic entropy, pointing towards a large spin-orbit coupling and orbital contribution in the system.

Design and syntheses of mono and multivalent mannosyl-lipoconjugates for targeted liposomal drug delivery.

PubMed

Štimac, Adela; Cvitaš, Jelena TrmĿiĿ; Frkanec, Leo; Vugrek, Oliver; Frkanec, Ruža

2016-09-10

Multivalent mannosyl-lipoconjugates may be of interest for glycosylation of liposomes and targeted drug delivery because the mannose specifically binds to C-type lectin receptors on the particular cells. In this paper syntheses of two types of novel O-mannosides are presented. Conjugates 1 and 2 with a COOH- and NH2-functionalized spacer and the connection to a lysine and FmocNH-PEG-COOH, are described. The coupling reactions of prepared intermediates 6 and 4 with a PEGylated-DSPE or palmitic acid, respectively, are presented. Compounds 5, mono-, 8, di- and 12, tetravalent mannosyl-lipoconjugates, were synthesized. The synthesized compounds were incorporated into liposomes and liposomal preparations featuring exposed mannose units were characterized. Carbohydrate liposomal quartz crystal microbalance based assay has been established for studying carbohydrate-lectin binding. It was demonstrated that liposomes with incorporated mannosyl-lipoconjugates were effectively recognized by Con A and have great potential to be used for targeted liposomal drug delivery systems. Copyright © 2016 Elsevier B.V. All rights reserved.

Structures and standard molar enthalpies of formation of a series of Ln(III)–Cu(II) heteronuclear compounds with pyrazine-2,3-dicarboxylic acid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Qi; Xie, Gang; Wei, Qing

2014-07-01

Fifteen lanthanide–copper heteronuclear compounds, formulated as [CuLn{sub 2}(pzdc){sub 4}(H{sub 2}O){sub 6}]·xH{sub 2}O (1–6(x=2), 8(x=3), 9–10(x=4)); [CuLn{sub 2}(pzdc){sub 4}(H{sub 2}O){sub 4}]·xH{sub 2}O (7, 12–13, 15(x=4), 14(x=5), 11(x=8)) (Ln(III)=La(1); Ce(2); Pr(3); Nd(4); Sm(5); Eu(6); Gd(7); Tb(8); Dy(9); Ho(10); Er(11); Tm(12); Yb(13); Lu(14); Y(15); H{sub 2}pzdc (C{sub 6}H{sub 4}N{sub 2}O{sub 4})=pyrazine-2,3-dicarboxylic acid) have been hydrothermally synthesized. All compounds were characterized by element analysis, IR spectroscopy, single-crystal X-ray diffraction and thermal analysis. X-ray diffraction analyses confirm that all compounds are isostructural and feature a 3D brick-like framework structure with (4.6{sup 2}){sub 2}(4{sup 2}.6{sup 2}.8{sup 2})(6{sup 3}){sup 2}(6{sup 5}.8){sub 2} topology. Using 1 mol cm{supmore » −3} HCl(aq) as calorimetric solvent, with an isoperibol solution–reaction calorimeter, the standard molar enthalpies of formation of all compounds were determined by a designed thermochemical cycle. In addition, solid state luminescence properties of compounds 5, 6, 8 and 9 were studied in the solid state. - Graphical abstract: According to Hess' rule, the standard molar enthalpies of formation of Ln–Cu heterometallic coordination compounds were determined by a designed thermochemical cycle. - Highlights: • Fifteen lanthanide–copper heteronuclear isostructural compounds. • Structurally characterization by IR, X-ray diffraction and thermal analysis. • The standard molar enthalpy of formation. • Isoperibol solution–reaction calorimetry.« less

Syntheses, crystal structure, and electronic properties of the five ABaMQ{sub 4} compounds RbBaPS{sub 4}, CsBaPS{sub 4}, CsBaVS{sub 4}, RbBaVSe{sub 4}, and CsBaVSe{sub 4}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mesbah, Adel; ICSM, UMR 5257 CEA / CNRS / UM / ENSCM, Site de Marcoule-Bâtiment 426, BP 17171, 30207 Bagnols-sur-Cèze Cedex; Prakash, Jai

Five new compounds belonging to the ABaMQ{sub 4} family were synthesized by solid-state chemistry at 1123 K. The compounds RbBaPS{sub 4}, CsBaPS{sub 4}, CsBaVS{sub 4}, RbBaVSe{sub 4}, and CsBaVSe{sub 4} are isostructural and have the TlEuPS{sub 4} structure type. They crystallize in space group D{sup 16}{sub 2h} – Pnma of the orthorhombic system. Their structure consists isolated MQ{sub 4} tetrahedra separated by A and Ba atoms to form a salt-like structure. Density Functional Theory (DFT) calculations of the electronic structures with the use of the HSE functional suggest that the compounds are semiconductors with calculated band gaps of 3.3 eVmore » (RbBaPS{sub 4}), 3.4 eV (CsBaPS{sub 4}), 2.3 eV (CsBaVS{sub 4}), and 1.6 eV (RbBaVSe{sub 4}). - Graphical abstract: General view of the ABaMQ{sub 4} structure down the a axis. - Highlights: • Five new ABaMQ{sub 4} compounds were synthesized by solid-state chemistry at 1123 K. • RbBaPS{sub 4}, CsBaPS{sub 4}, CsBaVS{sub 4}, RbBaVSe{sub 4}, and CsBaVSe{sub 4} have the TlEuPS{sub 4} structure type. • The compounds are semiconductors with calculated band gaps ranging from 1.6 to 3.4 eV.« less

Single Crystal X-ray Study of 6-Phenyl-4-( p-tolyl)pyridin-2(1 H)-one

NASA Astrophysics Data System (ADS)

Khajuria, Rajni; Sharma, Suresh; Kapoor, Kamal K.; Gupta, Vivek K.

2017-12-01

The title compound 6-phenyl-4-( p-tolyl)pyridin-2(1 H)-one was synthesized via one-pot, three component reaction of ( E)-1-phenyl-3-( p-tolyl)-2-propen-1-one, ethyl 2-nitroacetate and ammonium acetate in refluxing ethanol, as a shiny green crystalline solid in 83% yield. Its structure was characterized by spectral studies and unambiguously corroborated by X-ray diffraction crystallography. The crystals of title compound are monoclinic, sp. gr. P21/ n, a = 11.8346(7) Å, b = 13.4413(9) Å, c = 17.7626(10) Å, β = 99.479(5)°, and Z = 8. All the rings in molecule of the title compound are planar. Hydrogen interactions play significant role in stabilizing the crystal structure and the supramolecular aggregate of molecules is facilitated by strong N-H···O and C-H···O type of hydrogen interactions.

Li3Ge3Se6: the first ternary lithium germanium selenide with interesting ∞[Ge6Se12]n chains constructed by ethane-like [Ge2Se6]6- clusters.

PubMed

Li, Guangmao; Zhen, Ni; Chu, Yu; Zhou, Zhongxiang

2017-12-21

Li 3 Ge 3 Se 6 , the first compound of the ternary Li/Ge/Se system, has been synthesized. Note that interesting 1D ∞ [Ge 6 Se 12 ] n chains constructed by ethane-like [Ge 2 Se 6 ] 6- clusters were discovered in its structure. Investigations on the structures of all the [Ge 2 Se 6 ] 6- cluster-containing compounds have shown that only in Li 3 Ge 3 Se 6 are there 1D chains composed of [Ge 2 Se 6 ] 6- clusters, which result from the space limitation within the tunnels surrounded by LiSe 6 octahedra. Raman spectrum was obtained to demonstrate the existence of Ge-Ge bonds. UV-visible-NIR diffuse reflection spectrum showed an optical bandgap of 2.08 eV. Theoretical calculations based on first principles have also been performed for its band structure and density of states to analyze its structure-property relationship.

A series of Zn/Cd coordination polymers constructed from 1,4-naphthalenedicarboxylate and N-donor ligands: Syntheses, structures and luminescence sensing of Cr3+ in aqueous solutions

NASA Astrophysics Data System (ADS)

Hu, Dong-Cheng; Fan, Yan; Si, Chang-Dai; Wu, Ya-Jun; Dong, Xiu-Yan; Yang, Yun-Xia; Yao, Xiao-Qiang; Liu, Jia-Cheng

2016-09-01

A novel series of Zn/Cd coordination polymers based on H3L, namely, [Zn2(HL)2(bipy)2(H2O)6]n (1), [Zn(HL)(phen)]n (2), [Cd3L2(bbi)3]n (3), [Zn3L2(bbi)3]n (4) [(H3L =4-[(1-carboxynaphthalen-2-yl)oxy]phthalic acid, bipy =4,4‧-bipyridine, phen =1,10-phenanthroline, bbi =1,1‧-(1,4-butanediyl)bis(imidazole] have been successfully synthesized by solvothermal reaction. Compound 1 possesses two diverse 1D chains constructed by different bipy coligands, which were further connected to form a 3D supramolecular architecture by hydrogen bonding interactions. Compound 2 possesses a complicated 1D chain based on secondary building unit (SBU) with binuclear Zn cluster. Compounds 3 and 4 exhibit similar 2D→3D framework, which can be rationalized as (3,4,4)-connected 3D net with a Schläfli symbol of (63.8.102)2(63)2(64.8.10). In particular, compound 3 exhibited a high sensitivity for Cr3+ in aqueous solutions, which suggest that compound 3 is a promising luminescent probe for selectively sensing Cr3+.

Bioactive compounds synthesized by non-ribosomal peptide synthetases and type-I polyketide synthases discovered through genome-mining and metagenomics.

PubMed

Nikolouli, Katerina; Mossialos, Dimitris

2012-08-01

Non-ribosomal peptide synthetases (NRPS) and type-I polyketide synthases (PKS-I) are multimodular enzymes involved in biosynthesis of oligopeptide and polyketide secondary metabolites produced by microorganisms such as bacteria and fungi. New findings regarding the mechanisms underlying NRPS and PKS-I evolution illustrate how microorganisms expand their metabolic potential. During the last decade rapid development of bioinformatics tools as well as improved sequencing and annotation of microbial genomes led to discovery of novel bioactive compounds synthesized by NRPS and PKS-I through genome-mining. Taking advantage of these technological developments metagenomics is a fast growing research field which directly studies microbial genomes or specific gene groups and their products. Discovery of novel bioactive compounds synthesized by NRPS and PKS-I will certainly be accelerated through metagenomics, allowing the exploitation of so far untapped microbial resources in biotechnology and medicine.

Structural, electronic and magnetic properties of the series of double perovskites (Ca , Sr) 2 - xLaxFeIrO6

NASA Astrophysics Data System (ADS)

Bufaiçal, L.; Adriano, C.; Lora-Serrano, R.; Duque, J. G. S.; Mendonça-Ferreira, L.; Rojas-Ayala, C.; Baggio-Saitovitch, E.; Bittar, E. M.; Pagliuso, P. G.

2014-04-01

Polycrystalline samples of the series of double perovskites Sr2-xLaxFeIrO6 were synthesized. Their structural, electronic and magnetic properties were investigated by X-ray powder diffraction, Mössbauer spectroscopy, magnetic susceptibility, heat capacity and electrical resistivity experiments. The compounds crystallize in a monoclinic structure and were fitted in space group P21 / n, with a significant degree of Fe/Ir cationic disorder. As in Ca2-xLaxFeIrO6 the Sr-based system seems to evolve from an antiferromagnetic ground state for the end members (x=0.0 and x=2.0) to a ferrimagnetic order in the intermediate regions (x ~ 1). Since Mössbauer spectra indicate that Fe valence remains 3+ with doping, this tendency of change in the nature of the microscopic interaction could be attributed to Ir valence changes, induced by La3+ electrical doping. Upon comparing both Ca and Sr series, Sr2-xLaxFeIrO6 is more structurally homogenous and presents higher magnetization and transition temperatures. Magnetic susceptibility measurements at high temperatures on Sr1.2La0.8FeIrO6 indicate a very high ferrimagnetic Curie temperature TC ~ 700 K. For the Sr2FeIrO6 compound, electrical resistivity experiments under applied pressure suggest that this material might be a Mott insulator.

2:1 Charge disproportionation in perovskite-structure oxide La{sub 1/3}Ca{sub 2/3}FeO{sub 3} with unusually-high-valence Fe{sup 3.67+}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Haichuan; Hosaka, Yoshiteru; Seki, Hayato

La{sub 1/3}Ca{sub 2/3}FeO{sub 3} with unusually-high-valence Fe{sup 3.67+} was synthesized at a high pressure and high temperature. The compound crystallizes in a √2a×2a×√2a perovskite cell in which the La and Ca ions at the A site are disordered. At 217 K the Fe{sup 3.67+} shows charge disproportionation to Fe{sup 3+} and Fe{sup 5+} in a ratio of 2:1, and this disproportionation is accompanied by transitions in magnetic and transport properties. The charge-disproportionated Fe{sup 3+} and Fe{sup 5+} are arranged along the <111> direction of the cubic perovskite cell. The local electronic and magnetic environments of Fe in La{sub 1/3}Ca{sub 2/3}FeO{submore » 3} are quite similar to those of Fe in La{sub 1/3}Sr{sub 2/3}FeO{sub 3}, and the 2:1 charge disproportionation pattern of Fe{sup 3+} and Fe{sup 5+} in La{sub 1/3}Ca{sub 2/3}FeO{sub 3} is also the same as that in La{sub 1/3}Sr{sub 2/3}FeO{sub 3}. - Graphical abstract: The perovskite-structure oxide La{sub 1/3}Ca{sub 2/3}FeO{sub 3} with unusually-high-valence Fe{sup 3.67+} shows charge disproportionation to Fe{sup 3+} and Fe{sup 5+} in a ratio of 2:1, and the charge-disproportionated Fe{sup 3+} and Fe{sup 5+} are arranged along the <111> direction of the cubic perovskite cell. - Highlights: • La{sub 1/3}Ca{sub 2/3}FeO{sub 3} with unusually-high-valence Fe{sup 3.67+} was synthesized at a high pressure and high temperature. • At 217 K the Fe{sup 3.67+} shows charge disproportionation (CD) to Fe{sup 3+} and Fe{sup 5+} in a ratio of 2:1. • The charge-disproportionated Fe{sup 3+} and Fe{sup 5+} are arranged along the <111> direction of the cubic perovskite cell. • The disproportionation is accompanied by transitions in magnetic and transport properties.« less

Thiazolo[3,2-b]-1,2,4-triazole-5(6H)-one substituted with ibuprofen: novel non-steroidal anti-inflammatory agents with favorable gastrointestinal tolerance.

PubMed

Uzgören-Baran, Ayşe; Tel, Banu Cahide; Sarıgöl, Deniz; Oztürk, Elif İnci; Kazkayası, Inci; Okay, Gürol; Ertan, Mevlüt; Tozkoparan, Birsen

2012-11-01

In an effort to establish new candidates with improved analgesic and anti-inflammatory activities and lower ulcerogenic risk, a series of thiazolo[3,2-b]-1,2,4-triazole-5(6H)-one derivatives of ibuprofen were synthesized. All compounds were evaluated for their in vivo anti-inflammatory and analgesic activities in mice. Furthermore, the ulcerogenic risks of the compounds were determined. In general, none of the compounds represent a risk for developing stomach injury as much as observed in the reference drugs ibuprofen and indomethacin. The compounds carrying a 3-phenyl-2-propenylidene (1a), (biphenyl-4-yl)methylidene (1f) and (1-methylpyrrol-2-yl)methylidene (1n) at the 6th position of the fused ring have been evaluated as potential analgesic/anti-inflammatory agents without a gastrointestinal side effect. These new compounds, therefore, deserve further attention to develop new lead drugs. Copyright © 2012 Elsevier Masson SAS. All rights reserved.

Synthesis of a sugar-organometallic compound 1,1‧-difurfurylferrocene and its microwave preparation of carbon/iron oxide nanocomposite

NASA Astrophysics Data System (ADS)

Zhao, Shanyu; Cooper, Daniel C.; Xu, Haixun; Zhu, Pinghua; Suggs, J. William

2013-01-01

In order to synthesize a carbon-metal or metal oxide combination sphere, carbonaceous resource furfural 1 was introduced, which was nucleophilic treated with 1,1‧-dilithioferrocene 2 to form a sugar-organometallic compound: ferrocenyl monosaccharide derivative 1,1‧-difurfurylferrocene 3. 1,1‧-Difurfurylferrocene 3 can be hydrothermally treated in a microwave reactor to give 300-500 nm microspheres with the α-Fe2O3 or Fe3O4 nanocrystals formed on the surface, which may be favorable for new magnetic materials preparation or instead of iron with other metal ions, versatile carbon/metal composites will be possibly synthesized for catalysis, drug delivery and magnetic uses.

Influence of global and local distortion on magnetic properties of cubic La0.6Ba0.4-xCaxCoO3

NASA Astrophysics Data System (ADS)

Chang, Hong; Gao, Yu; Wu, Qiang; Dong, Xiaohua; Li, Yunfei; Pang, Yanbo

2015-12-01

The magnetic and structural study of the La0.6Ba0.4-xCaxCoO3 (x=0.0, 0.1, 0.2, 0.3, and 0.4) compounds with the lowest global or local distortion are studied. The compounds with x=0, 0.1, 0.2 and 0.3 is crystallized in the structure with the space group Pm-3m, and that with x=0.4 is Pnma. A ferromagnetic-like transition is observed and the Curie temperature, ranging from 235 K to 220 K, decreases slightly with the increasing Ca2+ content for x≤0.3, and the transition temperature is as low as 175 K with x=0.4. A hump, with the hump temperature slightly increase with the Ca2+ content, is observed in the thermal magnetization curves of all of the compounds at the ZFC state, and it is owing to the magnetic frustration because of the coexistence of the FM and the AFM interaction. Above the transition temperature, the magnetic susceptibility versus the temperature is fitted with the ferromagnetic Curie-Weiss law for the compounds with x≤0.3, and that with x=0.4 coincides with the ferrimagnetic Weiss-mean-field model. The absolute values of the exchange constants J1 in the compounds with x≤0.3 and those of J CO 3+CO 3+ ,J CO 3+CO4+ ,JCO4+CO4+ of La0.6Ca0.4CoO3 are deduced from the fitting. The results indicate that (i) the ferromagnetic exchange constants J1 increases with the Ca2+ content x≤0.3; (ii) the ferromagnetic interaction, JCo3+Co4+, plays a main role in the magnetic properties of La0.6Ca0.4CoO3; (iii) the antiferromagnetic interactions, JCo3+Co3+, JCo4+Co4+, are not negligible in the compound x=0.4. The unsaturated magnetization at 70 kOe and the high coercive field in the hysteretic magnetization curve supports the existence of the antiferromagnetic interaction, and the percentage of the antiferromagnetic domain is calculated.

Preparation of carbon nanoparticles and carbon nitride from high nitrogen compound

DOEpatents

Huynh, My Hang V [Los Alamos, NM; Hiskey, Michael A [Los Alamos, NM

2009-09-01

The high-nitrogen compound 3,6-di(azido)-1,2,4,5-tetrazine (DiAT) was synthesized by a relatively simple method and used as a precursor for the preparation of carbon nanospheres and nanopolygons, and nitrogen-rich carbon nitrides.

R{sub 4}Ir{sub 13}Ge{sub 9} (R=La, Ce, Pr, Nd, Sm) and RIr{sub 3}Ge{sub 2} (R=La, Ce, Pr, Nd): Crystal structures with nets of Ir atoms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yarema, Maksym; Swiss Federal Laboratories for Materials Science and Technology; Zaremba, Oksana

The crystal structures of the new ternary compounds Sm{sub 4}Ir{sub 13}Ge{sub 9} and LaIr{sub 3}Ge{sub 2} were determined and refined on the basis of single-crystal X-ray diffraction data. They belong to the Ho{sub 4}Ir{sub 13}Ge{sub 9} (oP52, Pmmn) and CeCo{sub 3}B{sub 2} (hP5, P6/mmm) structure types, respectively. The formation of isotypic compounds R{sub 4}Ir{sub 13}Ge{sub 9} with R=La, Ce, Pr, Nd, and RIr{sub 3}Ge{sub 2} with R=Ce, Pr, Nd, was established by powder X-ray diffraction. The RIr{sub 3}Ge{sub 2} (R=La, Ce, Pr, Nd) compounds exist only in as-cast samples and decompose during annealing at 800 Degree-Sign C with the formationmore » of R{sub 4}Ir{sub 13}Ge{sub 9}. The structure of Sm{sub 4}Ir{sub 13}Ge{sub 9} contains intersecting, slightly puckered nets of Ir atoms (4{sup 4})(4{sup 3}.6){sub 2}(4.6{sup 2}){sub 2} and (4{sup 4}){sub 2}(4{sup 3}.6){sub 4}(4.6{sup 2}){sub 2} that are perpendicular to [0 1 1] as well as to [0 -1 1] and [0 0 1]. The Ir atoms are surrounded by Ge atoms that form tetrahedra or square pyramids (where the layers intersect). The Sm and additional Ir atoms (in trigonal-planar coordination) are situated in channels along [1 0 0] (short translation vector). In the structure of LaIr{sub 3}Ge{sub 2} the Ir atoms form planar Kagome nets (3.6.3.6) perpendicular to [0 0 1]. These nets alternate along the short translation vector with layers of La and Ge atoms. - Graphical abstract: The crystal structures contain the nets of Ir atoms as main structural motif: R{sub 4}Ir{sub 13}Ge{sub 9} contains intersecting slightly puckered nets of Ir atoms, whereas in the structure of RIr{sub 3}Ge{sub 2} the Ir atoms form planar Kagome nets. Highlights: Black-Right-Pointing-Pointer The Ir-rich ternary germanides R{sub 4}Ir{sub 13}Ge{sub 9} (R=La, Ce, Pr, Nd, Sm) and RIr{sub 3}Ge{sub 2} (R=La, Ce, Pr, Nd) have been synthesized. Black-Right-Pointing-Pointer The RIr{sub 3}Ge{sub 2} compounds exist only in as-cast samples and decompose during annealing

Synthesis and NMR analysis of model compounds related to fucosylated chondroitin sulfates: GalNAc and Fuc(1 → 6)GalNAc derivatives.

PubMed

Vinnitskiy, Dmitry Z; Ustyuzhanina, Nadezhda E; Dmitrenok, Andrey S; Shashkov, Alexander S; Nifantiev, Nikolay E

2017-01-13

Unsubstituted and 6-O-α-L-fucosylated propyl 2-acetamido-2-deoxy-β-D-galactopyranosides and their selectively O-sulfated (both in GalNAc and Fuc units) derivatives were synthesized as model compounds representing the fragments of fucosylated chondroitin sulfates (FCS) from sea cucumbers. Per-O-acetylated 2-deoxy-2-N-phthalimido-D-glucopyranose was used as a key precursor for the preparation of all 2-acetamido-2-deoxy-D-galactopyranoside containing products. Attempts at 6-O-glycosylation of propyl 3-O-benzoyl-2-deoxy-2-N-phthalimido-D-galactoside by 2-O-benzyl-3,4-di-O-chloracetyl-L-fucosyl trichloracetimidate in the presence of TMSOTf gave a 1:1 mixture of the corresponding α- and β-isomeric disaccharides, while the use of structurally related fucosyl bromide donor with promotion by Bu 4 NBr led to the formation of desired α-isomeric disaccharide exclusively. Selective removal of orthogonal O-protections permitted subsequent O-sulfation both at the GalNAc and Fuc units. Further removal of blocking groups yielded the target products which were systematically studied by 1 H and 13 C NMR spectroscopy in order to determine the spectral effects of O-sulfation and α-L-fucosylation needed for the development of computer assisted structural analysis of natural FCS. Copyright © 2016 Elsevier Ltd. All rights reserved.

Ethyl 4-anilino-2,6-bis­(4-chloro­phen­yl)-1-phenyl-1,2,5,6-tetra­hydro­pyridine-3-carboxyl­ate

PubMed Central

Yu, Jianfeng; Tang, Shiming; Zeng, Jingbin; Yan, Zifeng

2013-01-01

The title compound, C32H28Cl2N2O2, was synthesized by a multicomponent reaction of 4-chloro­benzaldehyde, aniline and ethyl aceto­acetate. The central 1,2,5,6-tetra­hydro­pyridine ring exhibits a distorted boat conformation and the two chloro­phenyl rings attached to the central ring at positions 2 and 6 are oriented in opposite directions. The two O atoms of the eth­oxy­carbonyl group are involved in intra­molecular N—H⋯O and C—H⋯O hydrogen bonds. In the crystal, weak C—H⋯O hydrogen bonds link mol­ecules related by translation along the b axis into chains. PMID:23795109

46 CFR 151.50-6 - Motor fuel antiknock compounds.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 46 Shipping 5 2010-10-01 2010-10-01 false Motor fuel antiknock compounds. 151.50-6 Section 151.50... BARGES CARRYING BULK LIQUID HAZARDOUS MATERIAL CARGOES Special Requirements § 151.50-6 Motor fuel antiknock compounds. When transporting motor fuel antiknock compounds containing tetraethyl lead and...

46 CFR 151.50-6 - Motor fuel antiknock compounds.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 46 Shipping 5 2014-10-01 2014-10-01 false Motor fuel antiknock compounds. 151.50-6 Section 151.50... BARGES CARRYING BULK LIQUID HAZARDOUS MATERIAL CARGOES Special Requirements § 151.50-6 Motor fuel antiknock compounds. When transporting motor fuel antiknock compounds containing tetraethyl lead and...

46 CFR 151.50-6 - Motor fuel antiknock compounds.

Code of Federal Regulations, 2011 CFR

2011-10-01

... 46 Shipping 5 2011-10-01 2011-10-01 false Motor fuel antiknock compounds. 151.50-6 Section 151.50... BARGES CARRYING BULK LIQUID HAZARDOUS MATERIAL CARGOES Special Requirements § 151.50-6 Motor fuel antiknock compounds. When transporting motor fuel antiknock compounds containing tetraethyl lead and...

Electrochemical Study on Newly Synthesized Chlorocurcumin as an Inhibitor for Mild Steel Corrosion in Hydrochloric Acid

PubMed Central

Al-Amiery, Ahmed A.; Kadhum, Abdul Amir H.; Mohamad, Abu Bakar; Musa, Ahmed Y.; Li, Cheong Jiun

2013-01-01

A new curcumin derivative, i.e., (1E,4Z,6E)-5-chloro-1,7-bis(4-hydroxy-3-methoxyphenyl)hepta-1,4,6-trien-3-one (chlorocurcumin), was prepared starting with the natural compound curcumin. The newly synthesized compound was characterized by elemental analysis and spectral studies (IR, 1H-NMR and 13C-NMR). The corrosion inhibition of mild steel in 1 M HCl by chlorocurcumin has been studied using potentiodynamic polarization (PDP) measurements and electrochemical impedance spectroscopy (EIS). The inhibition efficiency increases with the concentration of the inhibitor but decreases with increases in temperature. The potentiodynamic polarization reveals that chlorocurcumin is a mixed-type inhibitor. The kinetic parameters for mild steel corrosion were determined and discussed. PMID:28788402

1-(Benzenesulfonyl)-1,5-dihydro-4,1-benzoxazepine as a new scaffold for the design of antitumor compounds.

PubMed

Cruz-López, Olga; Ramírez, Alberto; Navarro, Saúl A; García, María A; Marchal, Juan A; Campos, Joaquín M; Conejo-García, Ana

2017-07-01

Bozepinib is a potent and selective anticancer compound which chemical structure is made up of a benzofused seven-membered ring and a purine moiety. We previously demonstrated that the purine fragment does not exert antiproliferative effect per se. A series of 1-(benzenesulfonyl)-4,1-benzoxazepine derivatives were synthesized in order to study the influence of the benzofused seven-membered ring in the biological activity of bozepinib by means of antiproliferative, cell cycle and apoptosis studies. Our results show that the methyleneoxy enamine sulfonyl function is essential in the antitumor activity of the structures and thus, it is a scaffold suitable for further modification with a view to obtain more potent antitumor compounds.

Synthesis and anti-lung cancer activity of a novel arsenomolybdate compound

NASA Astrophysics Data System (ADS)

Zhu, Tian-Tian; Wang, Juan; Chen, Song-Hu

2017-12-01

The new compound based on Wells-Dawson-type arsenomolybdate: [{Cu10(pz)11Cl4}{As2IIIAs2VMo6VMo12VIO62}]·H2O (1) has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis, X-ray powder diffraction (XRPD), XPS spectroscopy and thermogravimetric analysis (TG). Compound 1 is consisted of two As caps Wells-dawson-type arsenomolybdate and {Cu10(py)11} complexes by chloride bridge. In addition, the antitumor effects of the title compound 1 were studied on three human lung cancer cells (A549, SK-LU-1 and SW1573). The results showed that compared with the positive reference drug carboplatin, compound 1 displayed efficient antitumor activity.

Synthesis, spectroscopic characterization, X-ray structure and DFT studies on 2,6-bis(1-benzyl-1H-benzo[d]imidazol-2-yl)pyridine.

PubMed

İnkaya, Ersin; Günnaz, Salih; Özdemir, Namık; Dayan, Osman; Dinçer, Muharrem; Çetinkaya, Bekir

2013-02-15

The title molecule, 2,6-bis(1-benzyl-1H-benzo[d]imidazol-2-yl)pyridine (C(33)H(25)N(5)), was synthesized and characterized by elemental analysis, FT-IR spectroscopy, one- and two-dimensional NMR spectroscopies, and single-crystal X-ray diffraction. In addition, the molecular geometry, vibrational frequencies and gauge-independent atomic orbital (GIAO) (1)H and (13)C NMR chemical shift values of the title compound in the ground state have been calculated using the density functional theory at the B3LYP/6-311G(d,p) level, and compared with the experimental data. The complete assignments of all vibrational modes were performed by potential energy distributions using VEDA 4 program. The geometrical parameters of the optimized structure are in good agreement with the X-ray crystallographic data, and the theoretical vibrational frequencies and GIAO (1)H and (13)C NMR chemical shifts show good agreement with experimental values. Besides, molecular electrostatic potential (MEP) distribution, frontier molecular orbitals (FMO) and non-linear optical properties of the title compound were investigated by theoretical calculations at the B3LYP/6-311G(d,p) level. The linear polarizabilities and first hyper polarizabilities of the molecule indicate that the compound is a good candidate of nonlinear optical materials. The thermodynamic properties of the compound at different temperatures were calculated, revealing the correlations between standard heat capacity, standard entropy, standard enthalpy changes and temperatures. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis, spectroscopic characterization, X-ray structure and DFT studies on 2,6-bis(1-benzyl-1H-benzo[d]imidazol-2-yl)pyridine

NASA Astrophysics Data System (ADS)

İnkaya, Ersin; Günnaz, Salih; Özdemir, Namık; Dayan, Osman; Dinçer, Muharrem; Çetinkaya, Bekir

2013-02-01

The title molecule, 2,6-bis(1-benzyl-1H-benzo[d]imidazol-2-yl)pyridine (C33H25N5), was synthesized and characterized by elemental analysis, FT-IR spectroscopy, one- and two-dimensional NMR spectroscopies, and single-crystal X-ray diffraction. In addition, the molecular geometry, vibrational frequencies and gauge-independent atomic orbital (GIAO) 1H and 13C NMR chemical shift values of the title compound in the ground state have been calculated using the density functional theory at the B3LYP/6-311G(d,p) level, and compared with the experimental data. The complete assignments of all vibrational modes were performed by potential energy distributions using VEDA 4 program. The geometrical parameters of the optimized structure are in good agreement with the X-ray crystallographic data, and the theoretical vibrational frequencies and GIAO 1H and 13C NMR chemical shifts show good agreement with experimental values. Besides, molecular electrostatic potential (MEP) distribution, frontier molecular orbitals (FMO) and non-linear optical properties of the title compound were investigated by theoretical calculations at the B3LYP/6-311G(d,p) level. The linear polarizabilities and first hyper polarizabilities of the molecule indicate that the compound is a good candidate of nonlinear optical materials. The thermodynamic properties of the compound at different temperatures were calculated, revealing the correlations between standard heat capacity, standard entropy, standard enthalpy changes and temperatures.

Structure of 18R shifted hexagonal perovskite La{sub 6}MgTi{sub 4}O{sub 18} revisited by neutron diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, Fengqi; Kuang, Xiaojun, E-mail: kuangxj@glut.edu.cn

The structure of 18-layer shifted B-site deficient hexagonal perovskite La{sub 6}MgTi{sub 4}O{sub 18} compound has been re-examined by neutron powder diffraction. Structural analysis reveals that La{sub 6}MgTi{sub 4}O{sub 18} compound adopts a 18R octahedral-tilted structure with LaO{sub 3} layer stacking sequence of (hhcccc){sub 3} in space group R{sup {sup -}}3, in contrast with the previously proposed R3m. La{sub 6}MgTi{sub 4}O{sub 18} demonstrates partially ordered Mg cation distribution with a preference on the central octahedral sites over the outer octahedral sites in the cubic perovskite blocks isolated by the single vacant octahedral layers between the two consecutive hexagonal layers. The instabilitymore » of the La{sub 6}MgTi{sub 4}O{sub 18} on alumina ceramic substrate at high temperature and its dependencies of cell parameters and permittivity were characterized as well. - Graphical abstract: 18-layer shifted hexagonal perovskite La{sub 6}MgTi{sub 4}O{sub 18} adopts octahedral-tilted structure in R{sup {sup -}}3 and demonstrates partially ordered Mg distribution in the cubic perovskite blocks isolated by the vacant octahedral layers. - Highlights: • Neutron diffraction reveals an octahedra-tilted structure in R{sup {sup -}}3 for La{sub 6}MgTi{sub 4}O{sub 18}. • Mg/Ti distribution in La{sub 6}MgTi{sub 4}O{sub 18} is partially ordered in the perovskite blocks. • Instability of La{sub 6}MgTi{sub 4}O{sub 18} on alumina ceramic at high temperature is demonstrated.« less

Linear Free Energy Relationships in Dinuclear Compounds. 2. Inductive Redox Tuning via Remote Substituents in Quadruply Bonded Dimolybdenum Compounds.

PubMed

Lin, Chun; Protasiewicz, John D.; Smith, Eugene T.; Ren, Tong

1996-10-23

Syntheses and characterizations are reported for dimolybdenum(II) compounds supported by the diarylformamidinate (ArNC(H)NAr(-)) ligand, where Ar is XC(6)H(4)(-), with X as p-OMe (1), H (2), m-OMe (3), p-Cl (4), m-Cl (5), m-CF(3) (6), p-COMe (7), p-CF(3) (8), or Ar is 3,4-Cl(2)C(6)H(3)(-) (9) or 3,5-Cl(2)C(6)H(3)(-) (10). The (quasi)reversible oxidation potentials measured for the Mo(2)(5+)/Mo(2)(4+) couple were found to correlate with the Hammett constant (sigma(X)) of the aryl substituents according to the following equation: DeltaE(1/2) = E(1/2)(X) - E(1/2)(H) = 87(8sigma(X)) mV. Molecular structure determinations of compounds 1, 2, 5, and 10 revealed an invariant core geometry around the Mo(2) center, with statistically identical Mo-Mo quadruple bond lengths of 2.0964(5), 2.0949[8], 2.0958(6), and 2.0965(5) Å, respectively. Magnetic anisotropies for compounds 1-10 estimated on the basis of (1)H NMR data were similar and unrelated to sigma(X). Similarity in UV-vis spectra was also found within the series, which, in conjunction with the features of both molecular structures and (1)H NMR spectra, was interpreted as the existence of a constant upper valence structure across the series. Results of Fenske-Hall calculations performed for several model compounds paralleled the experimental observations.

Molecular Syntheses of Extended Materials

NASA Astrophysics Data System (ADS)

Paley, Daniel W.

Bottom-up molecular synthesis is a route to chemically and crystallographically uniform polymers and solid-state materials. Through the use of molecular precursors, we gain atomic-level control of functionality and fine-tuning of the collective properties of materials. This dissertation presents two studies that demonstrate this approach. Ring-opening alkyne metathesis polymerization is a possible approach to monodisperse conjugated polymers, but its applications have been limited by difficult syntheses and high air sensitivity of known organometallic ROAMP initiators. We designed a dimeric, air-stable molybdenum alkylidyne with a tris(phenolate) supporting ligand. The precatalyst is activated by addition of methanol and polymerizes cyclooctynes with excellent chemical selectivity and functional group tolerance. The Nuckolls and Roy groups have introduced a new family of solid-state compounds synthesized from cobalt chalcogenide clusters Co6Q 8(PR3)6 and fullerenes. The first examples of these materials crystallized in superatom lattices with the symmetry of simple inorganic solids CdI2 (P-3m1) and NaCl (Fm-3m). This dissertation reveals that further members of the family feature extraordinary diversity of structure, including a pseudo-trigonal array of fulleride dimers in [Co 6Te8(PEt3)6]2[C140 ][C70]2 and a heterolayered van der Waals cocrystal [Co6Se8(PEt2phen)6][C 60]5. In addition to these unusual crystal structures, this dissertation presents a method for assigning redox states from crystallographic data in Co6Q8 clusters. Finally, a detailed guide to the collection and solution of single-crystal X-ray data is presented. The guide is intended for independent study by new crystallographers.

Chemistry of anti-AIDS and anticancer compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yan, S.

1992-01-01

Several types of prodrugs of 2[prime], 3[prime]-dideoxynucleosides were designed and synthesized for evaluation as anti-AIDS drugs. These prodrugs include 5[prime]-O-acyl-2[prime], 3[prime]-dideoxynucleosides, in which the acyl groups are derived from both aromatic and aliphatic acids, [alpha]-amino acids, diacylglycerol carbonic acids, and diacylglycerol carbamic acids. By applying the pyridium-dihydropyridine redox delivery system to deliver 2[prime], 3[prime]-dideoxynucleosides to the central nervous system, 1,4-dihydropyridine-2[prime], 3[prime]-dideoxy-inosine and -adenosine compounds were synthesized. 5[prime]-Esters of 2[prime], 3[prime]-dideoxyinosine and 2[prime], 3[prime]-dideoxyadenosine were evaluated for their activity against the HIV-1 virus and for delivery to the central nervous system (CNS). The isomerization, hydrolysis, and oxidation of alkyl 1,4-dihydro-N-methylpyridine-3-carboxylates weremore » studied by [sup 1]H and [sup 13]C NMR spectroscopy. Three intermediates, 1,4-dihydro-N-methylpyridine-3-carboxylic acid, alkyl (methyl or isopropyl) 1,6-dihydro-N-methylpyridine-3-carboxylate, and 1,6-dihydro-N-methylpyridine-3-carboxylic acid, were observed by [sup 1]H and [sup 13]C NMR spectroscopy, and their percentages in solution were determined. The structures of the 1,6-dihydropyridine intermediates were confirmed by comparison of the NMR spectra with those of an authentic model compound, methyl N-(4-chlorobenzyl)-1,6-dihydropyridine-3-carboxylate. The rate of hydrolysis of alkyl 1,4-dihydro-N-methylpyridine-3-carboxylates depends on the steric bulk of the O-alkyl group. A new type of 1,4-dihydropyridine drug delivery system with a three-carbon spacer group, 9-[2,3-di-O-acetyl-5-O-[3-(1,4-dihydro-N-methylpyridine-3-carboxamido)propionyl]-[beta]-D-arabinofuranosyl]adenine was designed, synthesized, and evaluated to deliver ara-ADA to the CNS for treatment of herpes encephalitis.« less

Synthesis and TFT Properties of Fluorenyl Cored Conjugated Compound for Organic Thin Film Transistors.

PubMed

Kim, You Geun; Shaik, Baji; Jang, Yong Ju; Park, Song Yi; Kim, Jin Young; Lee, Sang-Gyeong

2016-03-01

The 5,5'-(4,4'-(9,9-dioctyl-9H-fluorene-2,7-diyl)bis(4,1-phenylene))bis(2-hexylthieno[3,2-b]thiophene) FCBT (6) was synthesized by connecting the fluorenyl, thienothiophenyl and phenyl units. The compound was characterized by FT-IR, H1NMR, C13NMR and mass spectroscopy. The compound has shown good solubility and thermal stability over 417 degrees C. The compound has shown hole mobility of 4.76 x 10(-6) cm2Ns. The on-off ratio and threshold voltage were 7.5 x 10(2) and -8.26 V respectively.

Electrochemical Study on Newly Synthesized Chlorocurcumin as an Inhibitor for Mild Steel Corrosion in Hydrochloric Acid.

PubMed

Al-Amiery, Ahmed A; Kadhum, Abdul Amir H; Mohamad, Abu Bakar; Musa, Ahmed Y; Li, Cheong Jiun

2013-11-27

A new curcumin derivative, i.e. , (1E,4Z,6E)-5-chloro-1,7-bis(4-hydroxy-3-methoxyphenyl)hepta-1,4,6-trien-3-one (chlorocurcumin), was prepared starting with the natural compound curcumin. The newly synthesized compound was characterized by elemental analysis and spectral studies (IR, ¹H-NMR and 13 C-NMR). The corrosion inhibition of mild steel in 1 M HCl by chlorocurcumin has been studied using potentiodynamic polarization (PDP) measurements and electrochemical impedance spectroscopy (EIS). The inhibition efficiency increases with the concentration of the inhibitor but decreases with increases in temperature. The potentiodynamic polarization reveals that chlorocurcumin is a mixed-type inhibitor. The kinetic parameters for mild steel corrosion were determined and discussed.

Theoretical insights on the electron doping and Curie temperature in La-doped Sr2CrWO6.

PubMed

Wang, Jing; Meng, Jian; Wu, Zhijian

2011-11-30

The structure and electronic and magnetic properties of La(x)Sr(2-x)CrWO(6) (x = 0.0, 0.5, 1.0, 1.5, 2.0) were investigated by using the density functional theory. With the increase of La doping, the extra electrons are injected into W 5d orbitals, which makes the spin moments of W increase. In addition, the calculated Curie temperature and total magnetic moments decrease with the increase of the electron doping, in agreement with the experimental observation. This also means that the decrease of Curie temperature with the electron doping is intrinsic. Half metallic properties are obtained for x = 0.0, 0.5, 1.5, and 2.0, whereas for x = 1.0, the compound is semiconducting. Copyright © 2011 Wiley Periodicals, Inc.

Structural and dielectric properties of Ba{sub 2}LaSbO{sub 6} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumari, Premlata, E-mail: k.premlata1@gmail.com; Dutta, Alo; Sinha, T. P.

2014-04-24

The ceramic Ba{sub 2}LaSbO{sub 6} (BLS) is synthesized by the solid state reaction technique. The Rietveld refinement of X-ray diffraction pattern at room temperature shows Monoclinic P2{sub 1}/n space group symmetry with lattice parameter a = 6.0720 (0) Å, b = 6.1058 (3) Å, c = 8.6016 (6) Å and β =89.7091 ° (8). Dielectric study of sample has been performed in the temperature range from 30 °C to 300 °C in the frequency range 50 Hz to 1.1 MHz. Dielectric relaxation peaks are observed in the imaginary part of complex permittivity of the spectra. The frequency dependence of realmore » and imaginary parts of dielectric permittivity is analyzed using Cole-Cole model. The temperature dependent relaxation time is found to obey the Arrhenius law having activation energy 0.48 eV which indicates that the conduction mechanism in the materials may be due to polaron hopping based on electron carriers. The complex plane plots of BLS shows the presence of both grain and grain boundary effects. Conductivity spectra follow the power law.« less

Synthesis of Novel Chiral Sulfonamide-Bearing 1,2,4-Triazole-3-thione Analogs Derived from D- and L-Phenylalanine Esters as Potential Anti-Influenza Agents.

PubMed

Başaran, Eyüp; Karaküçük-Iyidoğan, Ayşegül; Schols, Dominique; Oruç-Emre, Emine Elçin

2016-06-01

Novel enantiopure 1,2,4-trizole-3-thiones containing a benzensulfonamide moiety were synthesized via multistep reaction sequence starting with D-phenylalanine methyl ester and L-phenylalanine ethyl ester as a source of chirality. The chemical structures of all compounds were characterized by elemental analysis, UV, IR, (1) H NMR, (13) C NMR, 2D NMR (HETCOR), and mass spectral data. All compounds were tested in vitro antiviral activity against a broad variety of DNA and RNA viruses and in vitro cytostatic activity against murine leukemia (L1210), human T-lymphocyte (CEM) and human cervix carcinoma (HeLa) cell lines. Although enantiopure 1,2,4-triazole-3-thione analogs in (R) configuration emerged as promising anti-influenza A H1N1 subtype in Madin Darby canine kidney cell cultures (MDCK), their enantiomers exhibited no activity. Especially compounds , , , , and (EC50 : 6.5, 6.1, 2.4, 1.6, 1.7 μM, respectively) had excellent activity against influenza A H1N1 subtype compared to the reference drug ribavirin (EC50 : 8.0 μM). Several compounds have been found to inhibit proliferation of L1210, CEM and HeLa cell cultures with IC50 in the 12-53 μM range. Compound and in (R) configuration were the most active compounds (IC50 : 12-22 μM for and IC50 : 19-23 μM for ). Chirality 28:495-513, 2016. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

The synthesis and structure of a chiral 1D aluminophosphate chain compound: d-Co(en) 3[AlP 2O 8]·6.5H 2O

NASA Astrophysics Data System (ADS)

Chen, Peng; Li, Jiyang; Yu, Jihong; Wang, Yu; Pan, Qinhe; Xu, Ruren

2005-06-01

A new chiral one-dimensional (1D) aluminophosphate chain compound [ d-Co(en) 3][AlP 2O 8]·6.5H 2O (designated AlPO-CJ22) has been hydrothermally synthesized by using the optically pure d-Co(en) 3I 3 complex as the template. Single-crystal structural analysis reveals that its structure is built up from alternating connection of AlO 4 and PO 2(=O 2) tetrahedra to form corner-shared Al 2P 2 four-membered ring (4-MR) chains. The d-Co(en) 33+ complex cations extended along the 2 1 screw axis interact with the inorganic chains through hydrogen-bonds of N⋯O atoms in a helical fashion. Optical rotation measurement shows that AlPO-CJ22 is chiral as with d-Co(en) 33+ complex cations. Crystal data: orthorhombic, I2 12 12 1, a=8.5573(8) Å, b=22.613(2) Å, c=22.605(2) Å, Z=8, R1=0.067, wR2=0.1291, and Flack parameter: -0.02(3). CCDC number: 254179.

The hunt for LaFeSbO: Synthesis of La{sub 2}SbO{sub 2} and a case of mistaken identity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Muir, Sean, E-mail: muirs@onid.orst.edu; Vielma, Jason, E-mail: vielmaj@onid.orst.edu; Schneider, Guenter, E-mail: guenter.schneider@oregonstate.edu

The phase La{sub 2}SbO{sub 2} has been identified and characterized in the course of our efforts to realize LaFeSbO, a composition of great interest to the superconductor community. The compound La{sub 2}SbO{sub 2} is a tetragonal layered oxypnictide containing La{sub 2}O{sub 2} layers similar to LaMPnO compositions (where M=transition metal, Pn=pnictide) separated by pnictide anion layers. In order to better understand why LaFeSbO has remained elusive, density functional theory calculations have been used to determine the ground state heats of formation for LaFeSbO, La{sub 2}SbO{sub 2}, and other competing phases within the La-Fe-Sb-O system, as well as the phonon spectrummore » for LaFeSbO. These efforts suggest that LaFeSbO is a potentially metastable composition. - Graphical abstract: The layered oxypnictide compounds La{sub 2}SbO{sub 2} and La{sub 1.9}Sr{sub 0.1}SbO{sub 2} have been synthesized and investigated. Both crystallize in a ThCr{sub 2}Si{sub 2} type configuration and are semiconducting. Stability of the unreported compound LaFeSbO has been investigated using density functional theory. A case of mistaken identity in the literature regarding the composition LaNiBiO is addressed. Highlights: Black-Right-Pointing-Pointer The composition La{sub 2}SbO{sub 2} has been identified. Black-Right-Pointing-Pointer La{sub 2}SbO{sub 2} belongs to an unusual group of materials containing Pn{sup 2-} anions. Black-Right-Pointing-Pointer La{sub 2}SbO{sub 2} and La{sub 1.9}Sr{sub 0.1}SbO{sub 2} are both found to be semiconducting. Black-Right-Pointing-Pointer DFT has been used to calculate heats of formation within the La-Fe-Sb-O system. Black-Right-Pointing-Pointer The phonon spectrum for LaFeSbO reveals no unstable lattice mode.« less

Correlation between microstructure and electrical transport properties of La0.7(Ba1-xCax)0.3MnO3 (x = 0 and 0.03) synthesized by sol-gel

NASA Astrophysics Data System (ADS)

Kurniawan, Budhy; Winarsih, Suci; Imaduddin, Agung; Manaf, Azwar

2018-03-01

In this paper, we reported the correlation of structure, microstructure, and electrical transport properties of polycrystalline La0.7(Ba1-xCax)0.3MnO3 (x = 0 and 0.03). The materials were synthesized by sol-gel method. These materials have interesting electronic and magnetic properties which are heavily affected by the degree of crystallographic mismatch between the La and Mn sites. By tuning these sites, the double exchange (DE) and Coulomb interactions among Mn ions can be artificially controlled. La0.7Ba0.3MnO3 is one of the strong candidates for application because it has high magnetoresistance and magnetocaloric properties. Doped Ca to the La0.7Ba0.3MnO3 is aimed for reducing its transition temperature to near room temperature and increasing the magnetoresistance and magnetocaloric properties of this material. Jahn-Teller distortion can be linked to core-shell model with the result of percolation model.

4-Functionalized 1,3-diarylpyrazoles bearing 6-aminosulfonylbenzothiazole moiety as potent inhibitors of carbonic anhydrase isoforms hCA I, II, IX and XII.

PubMed

SitaRam; Ceruso, Mariangela; Khloya, Poonam; Supuran, Claudiu T; Sharma, Pawan K

2014-12-15

A series of 24 novel heterocyclic compounds-functionalized at position 4 with aldehyde (5a-5f), carboxylic acid (6a-6f), nitrile (7a-7f) and oxime (8a-8f) functional groups-bearing 6-aminosulfonybenzothiazole moiety at position 1 of pyrazole has been synthesized and investigated for the inhibition of four isoforms of the α-class carbonic anhydrases (CAs, EC 4.2.1.1), comprising hCAs I and II (cytosolic, ubiquitous isozymes) and hCAs IX and XII (transmembrane, tumor associated isozymes). Against the human isozyme hCA I, compounds 6a-6f showed medium-weak inhibitory potential with Ki values in the range of 157-690nM with 6a showing better potential than the standard drug acetazolamide (AZA). Against hCA II, all the compounds showed excellent to moderate inhibition with Ki values of compounds 5a, 5d, 5f, 6a-6f, 8d and 8f lower than 12nM (Ki of AZA). Against hCA IX, all the compounds showed moderate inhibition with the exception of 6e which showed nearly 9 fold a better profile compared to AZA, whereas against hCA XII, four compounds 6e, 7a, 7b and 7d showed Ki in the same order as that of AZA. Carboxylic acid 6e was found to be an excellent inhibitor of both hCA IX and XII, with Ki values of 2.8nM and 5.5nM, respectively. Copyright © 2014 Elsevier Ltd. All rights reserved.

Synthesis of 7-hydroxy-4'-methoxyflavanone and 7-hydroxy-4'-methoxyflavone as a candidate anticancer against cervical (HeLa) cancer cell and colon (WiDr) cancer cell by in vitro

NASA Astrophysics Data System (ADS)

Matsjeh, Sabirin; Anwar, Chairil; Solikhah, Eti Nurwening; Farah, Harra Ismi; Nurfitria, Kurnia

2017-03-01

The compound 7-hydroxy-4'-methoxyflavanone and 7-hydroxy-4'-methoxyflavone have been synthesized through cyclization reaction of 2 ', 4'-dihydroxy-4-methoxychalcone (1,3-diphenyl-2-propene-1-one). The 2 ', 4'-dihydroxy-4-methoxychalcone were synthesized through Claisen-Schmidt condensation from 2,4-dihydroxyacetophenone and 4-methoxybenzaldehyde (anisaldehyde) in aqueous KOH as a catalyst in ethanol. The 7-hydroxy-4'-methoxyflavanone has been synthesized through cyclization reaction of 2 ', 4'-dihydroxy-4-methoxychalcone by Oxa-Michael addition reaction with sulfuric acid as a catalyst in ethanol. The 7-hydroxy-4'-methoxyflavone has been synthesized through oxidative cyclization reaction of 2 ', 4'-dihydroxy-4-methoxychalcone using I2 in DMSO as a catalyst with a mole ratio (1: 1) mol. All these producets were characterized by FT-IR, GC-MS, and 1H-NMR and 13C-NMR spectrometer. Both of these compounds were tested citotoxycity activity as an anticancer against cervical and colon cancer cells (HeLa and WiDr cell lines) using MTT assay in vitro. Dose series given test solution concentration on HeLa and WiDr cells starting from 0,78; 1,56; 3,12; 6,25; 12,50; 25; 50 and 100 µg/mL with a long incubation treatment for 24 hours. The results study showed that the 7-hydroxy-4'-methoxyflavanone as bright yellow crystals with a melting point 172-174 ° C and a yield of 56.67% and the 7-hydroxy-4'-methoxyflavone as bright yellow crystals with a yield of 88, 31%, and a melting point of 263-265 ° C. The test results cytotoxic 7-hydroxy-4-methoxyflavone showed active against HeLa cells with IC50 value of 25.73 µg/mL and was quite active in the WiDr cells with IC50 value of 83.75 µg/mL. The result of the activity of 7-hydroxy-4-methoxyflavanone show active cytotoxic activity against HeLa and WiDr cell growth with IC50 value of 40.13 µg/mL and 37.85 µg/mL. IC50 value indicated that 7-hydroxy-4'-methoxyflavone and 7-hydroxy-4'-methoxyflavanone potential as inhibitors in HeLa and

Synthesis of new 1,2,4-triazole compounds containing Schiff and Mannich bases (morpholine) with antioxidant and antimicrobial activities.

PubMed

Ünver, Yasemin; Deniz, Sadik; Çelik, Fatih; Akar, Zeynep; Küçük, Murat; Sancak, Kemal

2016-01-01

Compound 2 was synthesized by reacting CS 2 /KOH with compound 1. The treatment of compound 2 with hydrazine hydrate produced compound 3. Then, compound 3 was converted to Schiff bases (4a-d) by the handling with several aromatic aldehydes. The treatment of triazole compounds 4a-d containing Schiff base with morpholine gave compounds 5a-d. All compounds were tested for their antioxidant and antimicrobial activities. The antioxidant test results of DPPH• radical scavenging and ferric reducing/antioxidant power methods showed good antioxidant activity. The triazole-thiol (3) was the most active, and the effect of the substituent type of the thiophene ring on the activity was same for both Schiff bases (4a-d) and Mannich bases (5a-d). Among the newly synthesized triazole derivatives, the Schiff base 4d and the Mannich base 5d carrying nitro substituent on the thiophene ring showed promising antibacterial and antifungal activity, with lower MIC values than the standard antibacterial ampicillin.

Crystal Structure and Magnetic Properties of New Cubic Quaternary Compounds RT2Sn2Zn18 (R = La, Ce, Pr, and Nd, and T = Co and Fe)

NASA Astrophysics Data System (ADS)

Isikawa, Yosikazu; Mizushima, Toshio; Ejiri, Jun-ichi; Kitayama, Shiori; Kumagai, Keigou; Kuwai, Tomohiko; Bordet, Pierre; Lejay, Pascal

2015-07-01

The new cubic quaternary intermetallic compounds RT2Sn2Zn18 (R = La, Ce, Pr, and Nd, and T = Co and Fe) were synthesized by the mixture-metal flux method using Zn and Sn. The crystal structure was investigated by powder X-ray diffraction and with a four-circle X-ray diffractometer using single crystals. The space group of the compounds is Fdbar{3}m (No. 227). The rare-earth atom is at the cubic site which is the center of a cage composed of Zn and Sn atoms. The crystal structure is the same as the CeCr2Al20-type crystal structure except the atoms at the 16c site, i.e., the Zn atoms at the 16c site are completely replaced by Sn atoms, indicating that the compounds are crystallographically new ordered quaternary compounds. The lattice parameter a and the physical properties of the magnetic susceptibility χ, the magnetization M, and the specific heat C of these cubic caged compounds were investigated. LaCo2Sn2Zn18 and LaFe2Sn2Zn18 are enhanced Pauli paramagnets that originate from the Co and Fe itinerant 3d electrons. CeCo2Sn2Zn18 and CeFe2Sn2Zn18 are also enhanced Pauli paramagnets that originate from both the 3d electrons and Ce 4f electrons. PrCo2Sn2Zn18 and PrFe2Sn2Zn18 are nonmagnetic materials with huge values of C divided by temperature, which indicates that the ground state of Pr ions is a non-Kramers' doublet. NdCo2Sn2Zn18 and NdFe2Sn2Zn18 are magnetic materials with the Néel temperatures of 1.0 and 3.8 K, respectively. All eight compounds have large magnetic moments of Co/Fe in the paramagnetic temperature region, and thus their magnetic moments are inferred to be magnetically frustrating owing to the pyrochlore lattice in the low-temperature region.

Chiral halogenated Schiff base compounds: green synthesis, anticancer activity and DNA-binding study

NASA Astrophysics Data System (ADS)

Ariyaeifar, Mahnaz; Amiri Rudbari, Hadi; Sahihi, Mehdi; Kazemi, Zahra; Kajani, Abolghasem Abbasi; Zali-Boeini, Hassan; Kordestani, Nazanin; Bruno, Giuseppe; Gharaghani, Sajjad

2018-06-01

Eight enantiomerically pure halogenated Schiff base compounds were synthesized by reaction of halogenated salicylaldehydes with 3-Amino-1,2-propanediol (R or S) in water as green solvent at ambient temperature. All compounds were characterized by elemental analyses, NMR (1H and 13C), circular dichroism (CD) and FT-IR spectroscopy. FS-DNA binding studies of these compounds carried out by fluorescence quenching and UV-vis spectroscopy. The obtained results revealed that the ligands bind to DNA as: (Rsbnd ClBr) > (Rsbnd Cl2) > (Rsbnd Br2) > (Rsbnd I2) and (Ssbnd ClBr) > (Ssbnd Cl2) > (Ssbnd Br2) > (Ssbnd I2), indicating the effect of halogen on binding constant. In addition, DNA-binding constant of the Ssbnd and R-enantiomers are different from each other. The ligands can form halogen bonds with DNA that were confirmed by molecular docking. This method was also measured the bond distances and bond angles. The study of obtained data can have concluded that binding affinity of the ligands to DNA depends on strength of halogen bonds. The potential anticancer activity of ligands were also evaluated on MCF-7 and HeLa cancer cell lines by using MTT assay. The results showed that the anticancer activity and FS-DNA interaction is significantly dependent on the stereoisomers of Schiff base compounds as R-enantiomers displayed significantly higher activity than S-enantiomers. The molecular docking was also used to illustrate the specific DNA-binding of synthesized compounds and groove binding mode of DNA interaction was proposed for them. In addition, molecular docking results indicated that there are three types of bonds (Hsbnd and X-bond and hX-bond) between synthesized compounds and base pairs of DNA.

Promotion of hair growth by newly synthesized ceramide mimetic compound.

PubMed

Park, Bu-Mahn; Bak, Soon-Sun; Shin, Kyung-Oh; Kim, Minhee; Kim, Daehwan; Jung, Sang-Hun; Jeong, Sekyoo; Sung, Young Kwan; Kim, Hyun Jung

2017-09-09

Based on the crucial roles of ceramides in skin barrier function, use of ceramides or their structural mimetic compounds, pseudoceramides, as cosmetic ingredients are getting more popular. While currently used pseudoceramides are intended to substitute the structural roles of ceramides in stratum corneum, development of bioactive pseudoceramides has been repeatedly reported. In this study, based on the potential involvement of sphingolipids in hair cycle regulation, we investigated the effects of newly synthesized pseudoceramide, bis-oleamido isopropyl alcohol (BOI), on hair growth using cultured human hair follicles and animal models. BOI treatment promoted hair growth in cultured human hair follicles ex vivo and induced earlier conversion of telogen into anagen. Although we did not find a significant enhancement of growth factor expression and follicular cell proliferation, BOI treatment resulted in an increased sphinganine and sphingosine contents as well as increased ceramides contents in cultured dermal papilla (DP) cells. Taken together, our data strongly suggest that biologically active pseudoceramide promotes hair growth by stimulating do novo synthesis of sphingolipids in DP cells. Copyright © 2017 Elsevier Inc. All rights reserved.

New 1,3,4-thiadiazole compounds including pyrazine moiety: Synthesis, structural properties and antimicrobial features

NASA Astrophysics Data System (ADS)

Gür, Mahmut; Şener, Nesrin; Muğlu, Halit; Çavuş, M. Serdar; Özkan, Osman Emre; Kandemirli, Fatma; Şener, İzzet

2017-07-01

In the study, some new 1,3,4-thiadiazole compounds were synthesized and we have reported identification of the structures by using UV-Vis, FT-IR, 1H NMR, 13C NMR and Mass spectroscopic methods. Antimicrobial activities of the compounds against three microorganisms, namely, Candida albicans ATCC 26555, Staphylococcus aureus ATCC 9144, and Escherichia coli ATCC 25922 were investigated by using disk diffusion method. These thiadiazoles exhibited an antimicrobial activity against Staphylococcus aureus and Candida albicans. The experimental data was supported by the quantum chemical calculations. Density functional theory (DFT) calculations were carried out to obtain the ground state optimized geometries of the molecules using the B3LYP, M06 and PBE1PBE methods with 3-21 g, 4-31 g, 6-311++g(2d,2p), cc-pvtz and cc-pvqz basis sets in the different combinations. Frontier molecular orbitals (FMOs) energies, band gap energies and some chemical reactivity parameters were calculated by using the aforementioned methods and basis sets, and the results were also compared with the experimental UV-Vis data.

40 CFR 721.5356 - Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl]-omega...

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Ethanol, 2,2â²2â³-nitrilotris... Substances § 721.5356 Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl... subject to reporting. (1) The chemical substance identified as ethanol, 2,2′2″-nitrilotris-, compound with...

40 CFR 721.5356 - Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl]-omega...

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Ethanol, 2,2â²2â³-nitrilotris... Substances § 721.5356 Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl... subject to reporting. (1) The chemical substance identified as ethanol, 2,2′2″-nitrilotris-, compound with...

40 CFR 721.5356 - Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl]-omega...

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Ethanol, 2,2â²2â³-nitrilotris... Substances § 721.5356 Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl... subject to reporting. (1) The chemical substance identified as ethanol, 2,2′2″-nitrilotris-, compound with...

40 CFR 721.5356 - Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl]-omega...

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Ethanol, 2,2â²2â³-nitrilotris... Substances § 721.5356 Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl... subject to reporting. (1) The chemical substance identified as ethanol, 2,2′2″-nitrilotris-, compound with...

40 CFR 721.5356 - Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl]-omega...

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Ethanol, 2,2â²2â³-nitrilotris... Substances § 721.5356 Ethanol, 2,2′2″-nitrilotris-, compound with alpha-2,4,6-tris (1-phenylethyl)phenyl... subject to reporting. (1) The chemical substance identified as ethanol, 2,2′2″-nitrilotris-, compound with...

[miR-497 suppresses proliferation of human cervical carcinoma HeLa cells by targeting cyclin E1].

PubMed

Han, Jiming; Huo, Manpeng; Mu, Mingtao; Liu, Junjun; Zhang, Jing

2014-06-01

To evaluate the effect of miR-497 on proliferation of human cervical carcinoma HeLa cells and target relationship between miR-497 and cyclin E1 (CCNE1). Pre-miR-497 sequences were synthesized and cloned into pcDNATM6.2-GW to construct recombinant plasmid pcDNATM6.2-GW-pre-miR-497 and identified by real-time quantitative PCR (qRT-PCR). In addition, sequences of the wild-type CCNE1 (WT-CCNE1) and mutant CCNE1 (MT-CCNE1) were respectively cloned into pmirGLO vectors. MTT assay was used to explore the impact of miR-497 on the proliferation of HeLa cells. Furthermore, the target effect of miR-497 on the CCNE1 was identified by dual-luciferase reporter assay system, qRT-PCR and Western blotting. The recombinant plasmids pcDNATM6.2-GW-pre-miR-497 and pmirGLO-WT-CCNE1, pmirGLO-MT-CCNE1 were successfully constructed, and the miR-497 expression level in HeLa cells transfected with pre-miR-497 was significantly higher than that in the neg-miR group (P<0.05). MTT assay showed that miR-497 could significantly inhibit the proliferation of HeLa cells (P<0.05). A remarkable reduction of luciferase activities of WT-CCNE1 reporter was observed in HeLa cells with pre-miR-497 transfection (P<0.01), and the mRNA and protein expression levels of CCNE1 were down-regulated in HeLa cells transfected with pre-miR-497 (P<0.05). Over-expressed miR-497 in HeLa cells could suppress cell proliferation by targeting CCNE1.

Synthesis and antibacterial activity of bis-[2-hydroxy-3-(1,7,8,9,10-pentamethyl-3,5-dioxo-4-aza-tricyclo[5.2.1.0(2,6)]dec-8-en-4-yloxy)-propyl]-dimethyl-ammonium chloride.

PubMed

Struga, Marta; Kossakowski, Jerzy; Stefańska, Joanna; Zimniak, Andrzej; Koziol, Anna E

2008-06-01

A new quaternary ammonium compound, bis-[2-hydroxy-3-(1,7,8,9,10-pentamethyl-3,5-dioxo-4-aza-tricyclo[5.2.1.0(2,6)]dec-8-en-4-yloxy)-propyl]-dimethyl-ammonium chloride (4), was synthesized. The compound was investigated for antibacterial activity, including Gram-positive cocci and Gram-negative rods, and antifungal activity. Compound 4 showed significant inhibition against Staphylococcus aureus. Research was carried out over 4 standard strains and 40 hospital strains. Elementary analysis and/or MS, (1)H NMR and (13)C NMR spectra confirmed the identity of the products. The molecular structure of 3 was determined by an X-ray analysis.

Electronic, thermodynamics and mechanical properties of LaB6 from first-principles

NASA Astrophysics Data System (ADS)

Ivashchenko, V. I.; Turchi, P. E. A.; Shevchenko, V. I.; Medukh, N. R.; Leszczynski, Jerzy; Gorb, Leonid

2018-02-01

Up to date, the electronic structure properties of amorphous lanthanum hexaboride, a-LaB6, were not yet investigated, and the thermodynamic and mechanical properties of crystalline lanthanum hexaboride (c-LaB6) were studied incompletely. The goal of this work was to fill these gaps in the study of lanthanum hexaborides. The electronic and phonon structures, thermodynamic and mechanical properties of both crystalline and amorphous lanthanum hexaborides (c-LaB6, a-LaB6, respectively) were investigated within the density functional theory. An amorphyzation of c-LaB6 gives rise to the metal - semiconductor transition. The thermal conductivity decreases on going from c-LaB6 to a-LaB6. The elastic moduli, hardness, ideal tensile and shear strengths of a-LaB6 are significantly lower compared to those of the crystalline counterpart, despite the formation of the icosahedron-like boron network in the amorphous phase. For c-LaB6, the stable boron octahedrons are preserved after the failure under tensile and shear strains. The peculiarity in the temperature dependence of heat capacity, Cp(T), at 50 K is explained by the availability of a sharp peak at 100 cm-1 in the phonon density of states of c-LaB6. An analysis of the Fermi surface indicates that this peak is not related to the shape of the Fermi surface, and is caused by the vibration of lanthanum atoms. In the phonon spectrum of a-LaB6, the peak at 100 cm-1 is significantly broader than in the spectrum of c-LaB6, for which reason the anomaly in the Cp(T) dependence of a-LaB6 does not appear. The calculated characteristics are in good agreement with the available experimental data.

Synthese de champs sonores adaptative

NASA Astrophysics Data System (ADS)

Gauthier, Philippe-Aubert

La reproduction de champs acoustiques est une approche physique au probleme technologique de la spatialisation sonore. Cette these concerne l'aspect physique de la reproduction de champs acoustiques. L'objectif principal est l'amelioration de la reproduction de champs acoustiques par "synthese de champs acoustiques" ("Wave Field Synthesis", WFS), une approche connue, basee sur des hypotheses de champ libre, a l'aide du controle actif par l'ajout de capteurs de l'erreur de reproduction et d'une boucle fermee. Un premier chapitre technique (chapitre 4) expose les resultats d'appreciation objective de la WFS par simulations et mesures experimentales. L'effet indesirable de la salle de reproduction sur les qualites objectives de la WFS fut illustre. Une premiere question de recherche fut ensuite abordee (chapitre 5), a savoir s'il est possible de reproduire des champs progressifs en salle dans un paradigme physique de controle actif: cette possibilite fut prouvee. L'approche technique privilegiee, "synthese de champs adaptative" ("Adaptive Wave Field Synthesis" [AWFS]), fut definie, puis simulee (chapitre 6). Cette approche d'AWFS comporte une originalite en controle actif et en reproduction de champs acoustiques: la fonction cout quadratique representant la minimisation des erreurs de reproduction inclut une regularisation de Tikhonov avec solution a priori qui vient de la WFS. L'etude de l'AWFS a l'aide de la decomposition en valeurs singulieres (chapitre 7) a permis de comprendre les mecanismes propres a l'AWFS. C'est la deuxieme principale originalite de la these. L'algorithme FXLMS (LMS et reference filtree) est modifie pour l'AWFS (chapitre 8). Le decouplage du systeme par decomposition en valeurs singulieres est illustre dans le domaine du traitement de signal et l'AWFS basee sur le controle independant des modes de rayonnement est simulee (chapitre 8). Ce qui constitue la troisieme originalite principale de cette these. Ces simulations du traitement de signal

Lithium ethylene dicarbonate identified as the primary product of chemical and electrochemical reduction of EC in 1.2 M LiPF6/EC:EMC electrolyte.

PubMed

Zhuang, Guorong V; Xu, Kang; Yang, Hui; Jow, T Richard; Ross, Philip N

2005-09-22

Lithium ethylene dicarbonate ((CH2OCO2Li)2) was chemically synthesized and its Fourier transform infrared (FTIR) spectrum was obtained and compared with that of surface films formed on Ni after cyclic voltammetry (CV) in 1.2 M lithium hexafluorophosphate (LiPF6)/ethylene carbonate (EC):ethyl methyl carbonate (EMC) (3:7, w/w) electrolyte and on metallic lithium cleaved in-situ in the same electrolyte. By comparison of IR experimental spectra with that of the synthesized compound, we established that the title compound is the predominant surface species in both instances. Detailed analysis of the IR spectrum utilizing quantum chemical (Hartree-Fock) calculations indicates that intermolecular association through O...Li...O interactions is very important in this compound. It is likely that the title compound in the passivation layer has a highly associated structure, but the exact intermolecular conformation could not be established on the basis of analysis of the IR spectrum.

Three-chain B{sub 6n+14} cages as possible precursors for the syntheses of boron fullerenes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, Haigang, E-mail: luhg@sxu.edu.cn; Li, Si-Dian

Using the first principle methods, we proposed a series of three-chain boron cages B{sub 6n+14} (n = 1–12) which are mainly built by fusing three boron semi-double-rings. Their simple geometric structures (approximate D{sub 3} or C{sub 3} symmetry) facilitate their bottom-up syntheses from the hexagonal B{sub 7} and the double-chain boron clusters, such as B{sub 2}, B{sub 4}, B{sub 6}, B{sub 8}H{sub 2}, B{sub 10}H{sub 2}, B{sub 12}H{sub 2}, and the double ring B{sub 20}. The spherical shapes of these three-chain boron cages show that they could be taken as the possible precursors to further synthesize the boron fullerenes, suchmore » as B{sub 80}. Therefore, these three-chain boron cages provide a possible synthesis pathway of the boron fullerenes from the experimentally synthesized small planar boron clusters.« less

Hydrothermal synthesis, experimental and theoretical characterization of a novel cocrystal compound in the 2:1 stoichiometric ratio containing 6-methyluracil and dipicolinic acid

NASA Astrophysics Data System (ADS)

Eshtiagh-Hosseini, H.; Aghabozorg, H.; Mirzaei, M.; Beyramabadi, S. A.; Eshghi, H.; Morsali, A.; Shokrollahi, A.; Aghaei, R.

2011-05-01

This paper reports the hydrothermal synthesis, experimental and theoretical studies of a novel cocrystal compound in the 2:1 stoichiometric ratio of 6-methyluracil (6mu) and dipicolinic acid (pydcH 2) formulated as [6mu] 2[pydcH 2] (1), for the first time. DFT calculations were performed to access the most possible geometry of the title cocrystal compound. All calculations were carried out with the B3LYP hybrid density functional level and 6-311+G(d,p) basis sets. The vibrational frequencies together with the 1H and 13C NMR chemical shifts have been calculated on the fully optimized geometry of 1. The theoretical results are in good agreement with the experimental and solution data. The theoretical, solution, and experimental (elemental analysis, mass spectrometry, FTIR, 1H and 13C NMR spectroscopies) results confirmed our proposed structure for 1 in the 2:1 stoichiometric ratio of 6mu and pydcH 2, respectively. The protonation and equilibrium constants of 6mu and pydcH 2 and constituent systems were determined by potentiometric studies and the corresponding distribution diagrams depicted.

Nitrogen-rich salts of 5,5‧-bistetrazole-1,1‧-diolate: Syntheses, structures and properties

NASA Astrophysics Data System (ADS)

Yang, Ting; Zhang, Jian-Guo; Zhang, Zhi-Bin; Gozin, Michael

2018-03-01

A series of new nitrogen-rich energetic salts containing 1H,1‧H-[5,5‧-bitetrazole]-1,1‧-diol (BTO) anion and ethane-1,2-diaminium (1), 1-amino-1H-1,2,3-triazol-3-ium (2), 4-amino-4H-1,2,4-triazol-1-ium (3) and 4,5-diamino-4H-1,2,4-triazol-1-ium (4) cations were synthesized by direct salt formation or by metathesis strategy. The structures of energetic salts 1-4 were comprehensively characterized by elemental analysis, mass spectrometry, IR and NMR spectroscopies and by X-ray crystallography. DSC and TGA methods were used to study thermal properties of these salts. Additionally, the non-isothermal kinetic parameters and thermodynamic parameters were calculated by utilizing the Kissinger's and Ozawa-Doyle's methods. The enthalpies of formation for all target compounds in this study were calculated, and their sensitivity to mechanical impact and friction was tested according to BAM guidelines. We found these new energetic salts exhibit good thermal stability and have typical decomposition temperatures above 230 °C, except for the salt 2. All our salts have highly-positive enthalpies of formation (311.1-473.6 kJ mol-1) and are insensitive to impact and friction stimuli (>40 J, 120 N). With a high nitrogen-rich content, high enthalpy of formation, good thermostability and very low sensitivity to impact, some of these new salts may have a potential for application in the field of environmentally friendly insensitive energetic materials.

Electrode characteristics of nanocrystalline AB{sub 5} compounds prepared by mechanical alloying

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Z.; Chen, Z.; Zhou, D.

1998-10-01

Nanocrystalline LaNi{sub 5} and LaNi{sub 4.5}Si{sub 0.5} synthesized by mechanical alloying were used as negative materials for Ni-MH batteries. It was found that the electrodes prepared with the nanocrystalline powders had similar discharge capacities, better activation behaviors, and longer cycle lifetimes, compared with the negative electrode prepared with polycrystalline coarse-grained LaNi{sub 5} alloy. The properties of the electrodes prepared with these nanocrystalline materials were attributed to the structural characteristics of the compounds caused by mechanical alloying.

The synthesis and the luminescence properties of Sr2Ga3La1-xDyxGe3O14

NASA Astrophysics Data System (ADS)

Wang, Qiang; Mu, Zhongfei; Yang, Lurong; Zhang, Shaoan; Zhu, Daoyun; Yang, Yibin; Luo, Dongxiang; Wu, Fugen

2018-02-01

A series of Sr2Ga3La1-xDyxGe3O14 (x = 0, 0.015, 0.03, 0.045, 0.06, 0.075, 0.09) phosphors were synthesized by high temperature solid state reactions. X-ray diffraction analysis proves that single-phase Sr2Ga3La1-xDyxGe3O14 (0 ≤ x ≤ 0.09) has been obtained. The particle size of these powders is in the range from 1 to 3 μm. The host Sr2Ga3LaGe3O14 emits blue white light under the excitation of 260 nm ultraviolet light. Dy3+ doped samples can be effectively excited with near ultraviolet light and exhibit two emission bands in the blue (4F9/2 → 6H15/2) and yellow regions (4F9/2 → 6H13/2), which can form white light. Present research indicates that Dy3+ doped Sr2Ga3LaGe3O14 have the potential to be a single-phase full-color emitting phosphor.

Androgen Receptor Antagonists and Anti-Prostate Cancer Activities of Some Newly Synthesized Substituted Fused Pyrazolo-, Triazolo- and Thiazolo-Pyrimidine Derivatives

PubMed Central

Bahashwan, Saleh A.; Fayed, Ahmed A.; Ramadan, Mohamed A.; Amr, Abd El-Galil E.; Al-Harbi, Naif O.

2014-01-01

A series of substituted pyrazole, triazole and thiazole derivatives (2–13) were synthesized from 1-(naphtho[1,2-d]thiazol-2-yl)hydrazine as starting material and evaluated as androgen receptor antagonists and anti-prostate cancer agents. The newly synthesized compounds showed potent androgen receptor antagonists and anti-prostate cancer activities with low toxicity (lethal dose 50 (LD50)) comparable to Bicalutamide as reference drug. The structures of newly synthesized compounds were confirmed by IR, 1H-NMR, 13C-NMR, and MS spectral data and elemental analysis. The detailed synthesis, spectroscopic data, LD50 values and pharmacological activities of the synthesized compounds are reported. PMID:25421248

Crystalline and Electronic Structures and Magnetic and Electrical Properties of La-Doped Ca2Fe2O5 Compounds

NASA Astrophysics Data System (ADS)

Phan, T. L.; Tho, P. T.; Tran, N.; Kim, D. H.; Lee, B. W.; Yang, D. S.; Thiet, D. V.; Cho, S. L.

2018-01-01

Brownmillerite Ca2Fe2O5 has been observed to exhibit many outstanding properties that are applicable to ecotechnology. However, very little work on doped Ca2Fe2O5 compounds has been carried out to widen their application scope. We present herein a detailed study of the crystalline/geometric and electronic structures and magnetic and electrical properties of Ca2- x La x Fe2O5 ( x = 0 to 1) prepared by conventional solid-state reaction. X-ray diffraction patterns indicated that the compounds with x = 0 to 0.05 exhibited brownmillerite-type single phase. La doping with higher content ( x ≥ 0.1) stimulated additive formation of Grenier- (LaCa2Fe3O8) and perovskite-type (LaFeO3) phases. Extended x-ray absorption fine structure spectroscopy at the Fe K-edge and electron spin resonance spectroscopy revealed presence of Fe3+ in the parent Ca2Fe2O5 ( x = 0) and both Fe3+ and Fe4+ in the doped compounds ( x ≥ 0.05). The Fe4+ content tended to increase with increasing x. This stimulates ferromagnetic exchange interactions between Fe3+ and Fe4+ ions and directly influences the magnetic properties of Ca2- x La x Fe2O5. Electrical resistivity ( ρ) measurements in the temperature range of T = 20 K to 400 K revealed that all the compounds exhibit insulator behavior; the ρ( T) data for x ≥ 0.1 could be described based on the adiabatic small polaron hopping model.

Phosphorus-nitrogen compounds: Part 28. Syntheses, structural characterizations, antimicrobial and cytotoxic activities, and DNA interactions of new phosphazenes bearing vanillinato and pendant ferrocenyl groups

NASA Astrophysics Data System (ADS)

Tümer, Yasemin; Asmafiliz, Nuran; Kılıç, Zeynel; Hökelek, Tuncer; Yasemin Koç, L.; Açık, Leyla; Yola, Mehmet Lütfi; Solak, Ali Osman; Öner, Yağmur; Dündar, Devrim; Yavuz, Makbule

2013-10-01

The gradually Cl replacement reactions of spirocyclic mono (1 and 2) and bisferrocenyl cyclotriphosphazenes (3-5) with the potassium salt of 4-hydroxy-3-methoxybenzaldehyde (potassium vanillinate) gave mono (1a-5a), geminal (gem-1b-5b), non-geminal (cis-1b, cis-5b and trans-2b-5b), tri (1c-5c) and tetra-substituted phosphazenes (1d-5d). Some phosphazenes have stereogenic P-center(s). The chirality of 4c was verified using chiral HPLC column. Electrochemical behaviors were influenced only by the number of ferrocene groups, but not the length of the amine chains and the substituent(s). The structures of the new phosphazenes were determined by FTIR, MS, 1H, 13C and 31P NMR, HSQC and HMBC spectral data. The solid-state structures of cis-1b and 4d were examined by single crystal X-ray diffraction techniques. The twelve phosphazene derivatives were screened for antimicrobial activity and the compounds 5a, cis-1b and 2c exhibited the highest antibacterial activity against G(+) and G(-) bacteria. In addition, it was found that overall gem-1b inhibited the growth of Mycobacterium tuberculosis. The compounds 1d, 2d and 4d were tested in HeLa cancer cell lines. Among these compounds, 2d had cytotoxic effect on HeLa cell in the first 48 h. Moreover, interactions between compounds 2a, gem-1b, gem-2b, cis-1b, 2c, 3c, 4c, 5c, 1d, 2d and 4d, and pBR322 plasmid DNA were investigated.

Syntheses of cytotoxic novel arctigenin derivatives bearing halogen and alkyl groups on aromatic rings.

PubMed

Yamauchi, Satoshi; Wukirsari, Tuti; Ochi, Yoshiaki; Nishiwaki, Hisashi; Nishi, Kosuke; Sugahara, Takuya; Akiyama, Koichi; Kishida, Taro

2017-09-01

The new lignano-9,9'-lactones (α,β-dibenzyl-γ-butyrolactone lignans), which showed the higher cytotoxicity than arctigenin, were synthesized. The well-known cytotoxic arctigenin showed activity against HL-60 cells (EC 50 =12μM), however, it was inactive against HeLa cells (EC 50 >100μM). The synthesized (3,4-dichloro, 2'-butoxy)-derivative 55 and (3,4-dichloro, 4'-butyl)-derivative 66 bearing the lignano-9,9'-lactone structures showed the EC 50 values of 10μM and 9.4μM against HL-60 cells, respectively. Against HeLa cells, the EC 50 value of the derivative 66 was 27μM. By comparing the activities with the corresponding 9,9'-epoxy structure (tetrahydrofuran compounds), the importance of the lactone structure of 55 and 66 for the higher activities was shown. The substituents on the aromatic ring of the lignano-9,9'-lactones affected the cytotoxicity level, observing more than 10-fold difference. Copyright © 2017. Published by Elsevier Ltd.

Superconductivity in Cage Compounds LaTr2Al20 with Tr = Ti, V, Nb, and Ta

NASA Astrophysics Data System (ADS)

Yamada, Akira; Higashinaka, Ryuji; Matsuda, Tatsuma D.; Aoki, Yuji

2018-03-01

Electrical resistivity, magnetic susceptibility, and specific heat measurements on single crystals of LaTr2Al20 (Tr = Ti, V, Nb, and Ta) revealed that these four compounds exhibit weak-coupling superconductivity with transition temperatures Tc = 0.46, 0.15, 1.05, and 1.03 K, respectively. LaTi2Al20 is most probably a type-I superconductor, which is quite rare among intermetallic compounds. Single-crystal X-ray diffraction suggests "rattling" anharmonic large-amplitude oscillations of Al ions (16c site) on the Al16 cage, while no such feature is suggested for the cage-center La ion. Using a parameter dGFS quantifying the "guest free space" of the cage-center ion, we demonstrate that nonmagnetic RTr2Al20 superconductors are classified into two groups, i.e., (A) dGFS ≠ 0 and Tc correlates with dGFS, and (B) dGFS ≃ 0 and Tc seems to be governed by other factors.

Synthesis, characterization and biological activities of metal(II) dipicolinate complexes derived from pyridine-2,6-dicarboxylic acid and 2-(piperazin-1-yl)ethanol

NASA Astrophysics Data System (ADS)

Büyükkıdan, Nurgün; Yenikaya, Cengiz; İlkimen, Halil; Karahan, Ceyda; Darcan, Cihan; Korkmaz, Tülin; Süzen, Yasemin

2015-12-01

The new water-soluble and air stable compounds (H2ppz)[Co(dipic)2]·6H2O (1), (H2ppz)[Ni(dipic)2]·6H2O (2) and (H2ppz)[Zn(dipic)2]·6H2O (3) were prepared by the reaction of corresponding metal(II) acetates and a proton transfer salt, (H2ppz) (Hdipic)2, (4) of pyridine-2,6-dicarboxylic acid (H2dipic) and 2-(piperazin-1-yl)ethanol (ppz). The compounds 1-3 were characterized by elemental, IR, UV-vis. thermal analyses, magnetic measurement and single crystal X-ray diffraction studies. The molecular structures of the title compounds consist of one 1-(2-hydroxyethyl)piperazine-1,4-diium (H2ppz+2) cation, one bis(pyridine-2,6-dicarboxylate)metal(II) [M(dipic)2]2- anion, and six uncoordinated water molecules. In compounds 1-3 the metal ions coordinate to two oxygen and one nitrogen atoms of two pyridine-2,6-dicarboxylate molecules forming an octahedral environment. Antimicrobial activities against Gram (-) wild type (Escherichia coli and Pseudomonas aeruginosa), Gram (+) wild type (Staphylococcus aureus, Staphylococcus epidermidis, Bacillus cereus and Bacillus subtilis) and clinical isolate (Morganella morganii, Proteus vulgaris and Enterobacter aeruginosa) were also studied. The results were reported, discussed and compared with the corresponding starting materials ((H2ppz) (Hdipic)2 (4), H2dipic and ppz). MIC (Minimal Inhibition Concentration) values of the newly synthesized compounds were determined as 4000 μg/ml (except B. subtilis and clinical isolate E. aeruginosa, >4000 μg/ml).

Lanthanum cerate (La2Ce2O7): hydrothermal synthesis, characterization and optical properties

NASA Astrophysics Data System (ADS)

Khademinia, Shahin; Behzad, Mahdi

2015-03-01

La2Ce2O7 nano-powders were synthesized via a hydrothermal reaction in a deionized water (S 1) and in a 2 M NaOH aqueous solution (S 2) at 180 °C for 48 h. La(NO3)3·H2O and (NH4)2Ce(NO3)6 were used in the stoichiometric 1:1 La:Ce molar ratio as raw materials. The obtained materials were crystallized in a cubic crystal structure with space group. The synthesized materials were characterized by powder X-ray diffraction technique and Fourier-transform infrared spectroscopy. To investigate the effect of the basic solution on the morphology of the obtained materials, the morphologies of the synthesized materials were studied by field emission scanning electron microscopy technique. The technique showed that the morphology of La2Ce2O7 samples changed from grain to rod-like structure in presence of the basic solution. Cell parameter refinements showed that these parameters were larger for S2 than those for S 1. Photoluminescence and ultraviolet visible spectra of the synthesized nanomaterials were also investigated.

Structural, optical, and ferromagnetic characterization of Sm-doped LaOCl nanocrystalline synthesized by solvothermal route: Significant effect of hydrogen post treatment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dakhel, A.A.

Pure and Sm-doped lanthanum oxychloride (LaOCl) nanomaterials were synthesized by solvothermal route followed by a subsequent heat treatment process. The objective of the present work is to study and develop conditions required to create stable room-temperature ferromagnetic (RT-FM) properties in LaOCl. To achieve that aim, magnetic samarium Sm{sup 3+} ions were used as dopant sources for stable FM properties. Systematic structural, optical, and magnetic properties of undoped and Sm-doped LaOCl samples were investigated as function of post-annealing conditions (temperature and atmosphere). The optical absorption properties were studied by diffuse reflection spectroscopy (DRS). The magnetic measurements reveal that Sm-doped LaOCl nanopowdersmore » have partial RT-FM properties due to the doped ions. The variations of magnetic properties with pre-annealing temperature were investigated. Furthermore, the electronic medium of host LaOCl crystalline lattice, which carries the spin-spin (S.S) exchange interaction between localised dopant Sm{sup 3+}(4f{sup 5}) spins, was developed by annealing in hydrogen gas (hydrogenation). It was established that annealing in hydrogen atmosphere boosts the RT-FM properties so that the saturation magnetisation could be increased by more than 100%. Physical explanations and discussions were given in this paper. Thus, it was proved that the magnetic properties could be tailored to diamagnetic LaOCl compound by Sm-doping and post treatment under H{sub 2} atmosphere. Therefore, LaOCl nanocrystals could be used as a potential candidate for optical phosphor applications with magnetic properties. - Graphical abstract: M-H dependence of Sm-doped LaOCl powders. Study the effect of hydrogenation. - Highlights: • Synthesis of Sm-doped LaOCl nanoparticles. • DM LaOCl transforms to FM with dilute concentration of Sm doping. • Annealing under H{sub 2} atmosphere induces drastic boost in the FM properties. • Saturation magnetization attained

Structural Modifications of Neuroprotective Anti-Parkinsonian (−)-N6-(2-(4-(Biphenyl-4-yl)piperazin-1-yl)-ethyl)-N6-propyl-4,5,6,7-tetrahydrobenzo[d]thiazole-2,6-diamine (D-264): An Effort toward the Improvement of in Vivo Efficacy of the Parent Molecule

PubMed Central

2015-01-01

In our overall goal to develop multifunctional dopamine D2/D3 agonist drugs for the treatment of Parkinson’s disease (PD), we previously synthesized potent D3 preferring agonist D-264 (1a), which exhibited neuroprotective properties in two animal models of PD. To enhance the in vivo efficacy of 1a, a structure–activity relationship study was carried out. Competitive binding and [35S]GTPγS functional assays identified compound (−)-9b as one of the lead molecules with preferential D3 agonist activity (EC50(GTPγS); D3 = 0.10 nM; D2/D3 (EC50): 159). Compounds (−)-9b and (−)-8b exhibited high in vivo activity in two PD animal models, reserpinized and 6-hydroxydopamine (OHDA)-induced unilateral lesioned rats. On the other hand, 1a failed to show any in vivo activity in these models unless the compound was dissolved in 5–10% beta-hydroxy propyl cyclodextrin solution. Lead compounds exhibited appreciable radical scavenging activity. In vitro experiments with dopaminergic MN9D cells indicated neuroprotection by both 1a and (−)-9b from toxicity of MPP+. PMID:24471976

Design, synthesis and cytotoxicity of pyrano[4,3-b]indol-1(5H)-ones: A hybrid pharmacophore approach via gold catalyzed cyclization.

PubMed

Praveen, Chandrasekar; Ananth, D Babu

2016-05-15

Reported herein is the gold(III)-catalyzed 6-endo-dig cycloisomerization of 2-alkynyl-indole-3-carboxylic acids to form pyrano[4,3-b]indol-1(5H)-ones, which are pharmaceutically important structural motifs. The hitherto unknown substrates required for this methodology were conveniently synthesized in five steps with good overall yields. The utility of this new cycloisomerization is demonstrated by the excellent regioselectivity obtained using a range of substrates. The mildness of the method allowed functional group compatibility towards hydroxyl tether, displaying exquisite chemoselectivity. All the synthesized compounds were screened for their tumor cell growth inhibitory activity against human cervix adenocarcinoma (HeLa). Compound 7d emerged as the most active (IC50=0.69μM) among the tested series compared to the standard cis-platin (IC50=0.08μM). Copyright © 2016 Elsevier Ltd. All rights reserved.

1. Photocopy of photograph (original print on file at La ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

1. Photocopy of photograph (original print on file at La Grande District Office, La Grande, Oregon) No information about photographer or date OFFICE, SOUTHWEST FRONT - Union Ranger District Compound, Office, Fronting State Highway 203, at West edge of Union, Union, Union County, OR

Design, synthesis, and anti-HIV-1 activity of 1-aromatic methyl-substituted 3-(3,5-dimethylbenzyl)uracil and N-3,5-dimethylbenzyl-substituted urea derivatives

PubMed Central

Sakakibara, Norikazu; Baba, Masanori; Okamoto, Mika; Toyama, Masaaki; Demizu, Yosuke; Misawa, Takashi; Kurihara, Masaaki; Irie, Kohji; Kato, Yoshihisa; Maruyama, Tokumi

2015-01-01

Background A new series of 1-aromatic methyl-substituted 3-(3,5-dimethylbenzyl)uracil and N-3,5-dimethylbenzyl-substituted urea derivatives were synthesized and evaluated as non-nucleoside HIV-1 reverse transcriptase inhibitors. Methods A series of new 6-azido and 6-amino derivatives of 1-substituted-3-(3,5-dimethylbenzyl)uracils were synthesized using our previously reported method, and three acyclic derivatives were synthesized from urea. The anti-HIV-1 activities of these compounds were determined based on the inhibition of virus-induced cytopathogenicity in MT-4 cells. The cytotoxicities of the compounds were evaluated using the viability of mock-infected cells. Results Some of these compounds showed good-to-moderate activities against HIV-1 with half maximal effective concentration (EC50) values in the submicromolar or subnanomolar range. Compared with emivirine, compound 6-amino-3-(3,5-dimethylbenzyl)-1-(4-aminobenzyl)uracil showed significant anti-HIV-1 activity with an EC50 value of 10 nM and a high selectivity index of 1923. Preliminary structure–activity relationship studies and molecular modeling analyses were carried out to explore the major interactions between HIV-1 reverse transcriptase and the potent inhibitor 6-amino-3-(3,5-dimethylbenzyl)-1-(4-aminobenzyl)uracil; these results may be important for further development of this class of compounds as anti-HIV-1 agents. Conclusion The excellent activity of 6-amino-3-(3,5-dimethylbenzyl)-1-(4-aminobenzyl)uracil (EC50: 0.010 ± 0.006 µM, SI: >1923) may serve as the basis for conducting further investigations on the behavior of this class of compounds against drug-resistant mutants. PMID:26149262