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Sample records for 2 3 4

  1. 2,3,4,6-Tetrachlorophenol

    Integrated Risk Information System (IRIS)

    2,3,4,6 - Tetrachlorophenol ; CASRN 58 - 90 - 2 Human health assessment information on a chemical substance is included in the IRIS database only after a comprehensive review of toxicity data , as outlined in the IRIS assessment development process . Sections I ( Health Hazard Assessments for Noncar

  2. AgCo3PO4(HPO4)2.

    PubMed

    Guesmi, Abderrahmen; Driss, Ahmed

    2002-01-01

    The structure of the hydrothermally synthesized compound AgCo3PO4(HPO4)2, silver tricobalt phosphate bis(hydrogen phosphate), consists of edge-sharing CoO6 chains linked together by the phosphate groups and hydrogen bonds. The three-dimensional framework delimits two types of tunnels which accommodate Ag+ cations and OH groups. The title compound is isostructural with the compounds AM3H2(XO4)3 (A = Na or Ag, M = Co or Mn, and X = P or As) of the alluaudite structure type.

  3. Rapid, Microwave Accelerated Synthesis of [1,2,4]Triazolo[3,4-b][1,3,4]oxadiazoles from 4-Acylamino-1,2,4-Triazoles.

    PubMed

    Breunig, Stesphanie L; Olson, Margaret E; Harki, Daniel A

    2016-09-07

    1,2,4-Triazoles and 1,3,4-oxadiazoles are prevalent moieties in pharmaceutical agents, yet fused [1,2,4]-triazolo[3,4-b][1,3,4]oxadiazoles are surprisingly under-represented for both synthesis and biological application. We report a rapid, two-step synthesis of [1,2,4]-triazolo[3,4-b][1,3,4]oxadiazoles from commercial 4-amino-1,2,4-triazoles that is highlighted by a microwave accelerated intramolecular cyclization to generate the fused ring system. Our efforts to optimize reaction conditions and elucidate reaction mechanism are also described.

  4. Synthesis of 3-cyano-4-aryl-5-ethoxycarbonyl-6-methyl-3,4-dihydropyridine-2-thiones

    SciTech Connect

    Krauze, A.A.; Liepin'sh, E.E.; Pelcher, Yu.E.; Kalme, Z.A.; Dipan, I.V.; Dubur, G.Ya.

    1985-12-01

    The condensation of ethyl arylidenacetoacetate with cyanothioacetamide and of arylidenecyanothioacetamides with ethyl acetoacetate or of arylidenecyanothioacetamides with ethyl ..beta..-aminocrotonate gave 3-cyano-4-aryl-5-ethoxycarbonyl-6-methyl-3,4-dihydropyridine-2-thiones. PMR spectroscopy showed that the 3-cyano-4-aryl-3,4-dihydro-pyridine-2-thiones are formed as a mixture of cis and trans isomers.

  5. New 2-aryl-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidin-4-one derivatives as diuretics.

    PubMed

    Monge, A; Martinez-Merino, V; Simon, M A; Sanmartin, C

    1993-12-01

    2-Aryl-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidin-4-one derivatives having various substituents at the 4'-position, H or methyl at 1,3-positions and nitro or amino at 6-position were prepared and tested for their diuretic, natriuretic and kaliuretic activities on male Wistar rats at a dosage of 25 mg/kg or less. 2-(3-Pyridyl) derivatives were inactive. 1,3-Dimethyl-6-nitro-2-phenyl derivatives (1) were active depending on the electronic character of the 4'-substituent but at the same time were sodium-sparing. However, 1(H),3(H)-6-nitro-2-phenyl derivatives (2) were generally inactive as diuretics but active as potassium-sparing drugs. 6-Amino-1(H),3(H)-2-phenyl derivatives (4) were active as diuretics depending on dipolar moment of the substituent at the 4'-position, and induced moderate potassium release. The 6-amino-2-(4-trifluoromethylphenyl)-1, 2,3,4-tetrahydropyrido [2,3-d]pyrimidin-4-one (4f) remained active up to a dosage of 3 mg/kg. The structure-activity relationships were carried out in light of the adaptative least squares (ALS) method and discriminant functions for diuretic compounds were established.

  6. (3R,4S)-3,4-Isopropylidenedioxy-5-phenylsulfonylmethyl-3,4-dihydro-2H-pyrrole 1-oxide

    PubMed Central

    Flores, Mari Fe; Garcia, P.; M. Garrido, Narciso; Sanz, Francisca; Diez, David

    2011-01-01

    The title compound, C14H17NO5S, was prepared by oxidation of (2R,3S,4R)-2-phenyl­sulfonyl­methyl-1-hy­droxy-3,4-iso­pro­pyl­idene­dioxy­pyrrolidine. Its crystal structure confirms unequivocally its configuration. Two inter­molecular C—H⋯O inter­actions help to establish the packing. PMID:21754431

  7. A novel dilithiation approach to 3,4-dihydro-2H-1,3-benzothiazines, 3,4-Dihydro-2H-1,3-benzoxazines, and 2,3,4,5-tetrahydro-1,3-benzothiazepines.

    PubMed

    Katritzky, Alan R; Xu, Yong-Jiang; Jain, Ritu

    2002-11-15

    3,4-Dihydro-2H-1,3-benzothiazines 4, 3,4-dihydro-2H-1,3-benzoxazines 9, and 2,3,4,5-tetrahydro-1,3-benzothiazepines 6 were synthesized by directed ortho-lithiation of thiophenols and phenols and by side-chain lithiation of substituted thiophenols, respectively, in one-pot by reacting with N,N-bis[(benzotriazol-1-yl)methyl]amines 3 as 1,3-biselectrophile synthons.

  8. [Species differences in the in vitro metabolism of 2,4,5,2',3',4'-hexachlorobiphenyl].

    PubMed

    Koga, N; Kanamaru, T; Oishi, N; Kato, Y; Kimura, R; Haraguchi, K; Masuda, Y

    2001-05-01

    In vitro Metabolism of 2,4,5,2',3',4'-hexachlorobiphenyl (CB138) was studied using liver microsomes from rats, hamsters and guinea pigs. Guinea pig liver microsomes formed four metabolites named as M-1, M-2, M-3 and M-4 and these metabolites were all increased to about 4-5 fold of untreated microsomes by pretreatment of phenobarbital. Liver microsomes of rats and hamsters showed much less activity to metabolize CB138 than those of guinea pigs. Only phenobarbital-treated microsomes produced very small amounts of M-3 in rats and M-1, M-2 and M-3 in hamsters, but untreated and MC-treated microsomes did not. When mass spectra of the methylated derivatives of M-1, M-2, M-3 and M-4 were measured in GC/MS, the former two possess the molecular ion of 354 and the latter two had the molecular ion of 388. In addition, the mass fragmentation pattern indicated that M-1, M-2, M-3 and M-4 are 2-OH-4,5,2',3',4'-pentachlorobiphenyl, 5-OH-2,4,2',3',4'-pentachlorobiphenyl, 3-OH-CB138 and 2-OH-3,4,5,2',3',4'-hexachlorobiphenyl, respectively. Of four metabolites, the chemical structures of M-3 and M-4 were supported by the synthesized authentic compounds. From these results, it is suggested that the metabolism of CB138 in guinea pig liver proceeds mainly via 2,3-epoxide as an intermediate and a PB-inducible P450, CYP2B18, is the most important isozyme in CB138 metabolism.

  9. 5,4,3,2,...Thumbs Up!

    ERIC Educational Resources Information Center

    Brannon, Frank

    1997-01-01

    Presents activities for K-4 students that explore two areas of body mechanics--bones and joints--with an emphasis on the human hand. Relates knowledge of how the body functions to comparable examples in robotics such as the "hand" of the Canadarm of the space shuttle. Activities are geared for students in pairs. (AIM)

  10. Synthesis and Antibacterial Activity of 3-(Substituted)-2-(4-oxo-2-phenylquinazolin-3(4H)-ylamino)quinazolin-4(3H)-one.

    PubMed

    Appani, Ramgopal; Bhukya, Baburao; Gangarapu, Kiran

    2016-01-01

    A series of novel 3-(substituted)-2-(substituted quinazolinylamino)quinazolin-4(3H)-ones were synthesized by the reaction of 3-(substituted)-2-hydrazino-quinazoline-4(3H)-ones with 2-phenyl-3,1-benzoxazin-4-one. The starting materials 3-(substituted)-2-hydrazino-quinazolin-4(3H)-ones were synthesized from various primary amines by a multistep synthesis. All the title compounds were tested for their antibacterial activity using ciprofloxacin as reference standard. Compounds 3-(4-fluorophenyl)-2-(4-oxo-2-phenylquinazolin-3(4H)-ylamino)quinazolin-4(3H)-one (9a) and 3-(4-chlorophenyl)-2-(4-oxo-2-phenylquinazolin-3(4H)-ylamino)quinazolin-4(3H)-one (9h) emerged as the most active compounds of the series. These compounds have shown most potent antibacterial activity against the tested organisms of Proteus vulgaris and Bacillus subtilis having zone of inhibition values of 1.1 cm and 1.4 cm for compound 9a 1.2 cm and 1.0 cm for compound 9h, respectively.

  11. Synthesis and Antibacterial Activity of 3-(Substituted)-2-(4-oxo-2-phenylquinazolin-3(4H)-ylamino)quinazolin-4(3H)-one

    PubMed Central

    Appani, Ramgopal; Bhukya, Baburao; Gangarapu, Kiran

    2016-01-01

    A series of novel 3-(substituted)-2-(substituted quinazolinylamino)quinazolin-4(3H)-ones were synthesized by the reaction of 3-(substituted)-2-hydrazino-quinazoline-4(3H)-ones with 2-phenyl-3,1-benzoxazin-4-one. The starting materials 3-(substituted)-2-hydrazino-quinazolin-4(3H)-ones were synthesized from various primary amines by a multistep synthesis. All the title compounds were tested for their antibacterial activity using ciprofloxacin as reference standard. Compounds 3-(4-fluorophenyl)-2-(4-oxo-2-phenylquinazolin-3(4H)-ylamino)quinazolin-4(3H)-one (9a) and 3-(4-chlorophenyl)-2-(4-oxo-2-phenylquinazolin-3(4H)-ylamino)quinazolin-4(3H)-one (9h) emerged as the most active compounds of the series. These compounds have shown most potent antibacterial activity against the tested organisms of Proteus vulgaris and Bacillus subtilis having zone of inhibition values of 1.1 cm and 1.4 cm for compound 9a 1.2 cm and 1.0 cm for compound 9h, respectively. PMID:27190676

  12. Synthesis and COX-2 Inhibitory Activity of 4-[(E)-2-(4-Oxo-3-phenyl-3,4-dihydroquinazolin-2-yl)ethenyl]benzene-1-sulfonamideand Its Analogs

    PubMed Central

    Hayun; Hudiyono, Sumi; Hanafi, Muhammad; Yanuar, Arry

    2012-01-01

    Some novel 3-phenyl-2-[(E)-2-phenylethenyl]-3,4-dihydroquinazolin-4-one derivatives possessing para-sulfonamides groups on the phenyl ring of the 2-phenylethenyl moiety have been synthesized and their COX-2 inhibitory activity evaluated. The stuctures of the synthesized compounds were confirmed on the basis of FT-IR, 1H-NMR, 13C-NMR and mass spectral data. The COX-2 inhibition screening assay revealed that 4-[(E)-2-{3-(4-methoxyphenyl)-4-oxo-3,4-dihydroquinazolin-2-yl}ethenyl]benzene-1-sulfonamide had a maximum COX-2 inhibition (47.1%), at a concentration of 20 μM. PMID:24281337

  13. 40 CFR 721.5279 - 2,7-Naphthalenedisulfonic acid, 4-amino-3-[[42-amino-4-[(3-butoxy-2-hydroxypropyl)amino]phebyl...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Substances § 721.5279 2,7-Naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3,3′-dimethyl -4-yl]azo]-5... reporting. (1) The chemical substance identified as 2,7-naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3... 40 Protection of Environment 30 2010-07-01 2010-07-01 false 2,7-Naphthalenedisulfonic acid,...

  14. 40 CFR 721.5279 - 2,7-Naphthalenedisulfonic acid, 4-amino-3-[[42-amino-4-[(3-butoxy-2-hydroxypropyl)amino]phebyl...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... Substances § 721.5279 2,7-Naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3,3′-dimethyl -4-yl]azo]-5... reporting. (1) The chemical substance identified as 2,7-naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3... 40 Protection of Environment 31 2011-07-01 2011-07-01 false 2,7-Naphthalenedisulfonic acid,...

  15. 40 CFR 721.5279 - 2,7-Naphthalenedisulfonic acid, 4-amino-3-[[42-amino-4-[(3-butoxy-2-hydroxypropyl)amino]phebyl...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... Substances § 721.5279 2,7-Naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3,3′-dimethyl -4-yl]azo]-5... reporting. (1) The chemical substance identified as 2,7-naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3... 40 Protection of Environment 32 2013-07-01 2013-07-01 false 2,7-Naphthalenedisulfonic acid,...

  16. 40 CFR 721.5279 - 2,7-Naphthalenedisulfonic acid, 4-amino-3-[[42-amino-4-[(3-butoxy-2-hydroxypropyl)amino]phebyl...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... Substances § 721.5279 2,7-Naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3,3′-dimethyl -4-yl]azo]-5... reporting. (1) The chemical substance identified as 2,7-naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3... 40 Protection of Environment 31 2014-07-01 2014-07-01 false 2,7-Naphthalenedisulfonic acid,...

  17. 40 CFR 721.5279 - 2,7-Naphthalenedisulfonic acid, 4-amino-3-[[42-amino-4-[(3-butoxy-2-hydroxypropyl)amino]phebyl...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... Substances § 721.5279 2,7-Naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3,3′-dimethyl -4-yl]azo]-5... reporting. (1) The chemical substance identified as 2,7-naphthalenedisulfonic acid, 4-amino-3- phebyl]azo]-3... 40 Protection of Environment 32 2012-07-01 2012-07-01 false 2,7-Naphthalenedisulfonic acid,...

  18. 4 CFR 3.2 - Oath of office.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 4 Accounts 1 2010-01-01 2010-01-01 false Oath of office. 3.2 Section 3.2 Accounts GOVERNMENT ACCOUNTABILITY OFFICE PERSONNEL SYSTEM EMPLOYMENT § 3.2 Oath of office. The provisions of subchapter II of chapter 33 of title 5, U.S. Code, and Office of Personnel Management implementing regulations apply...

  19. Na3Al(AsO4)2

    PubMed Central

    Fakhar Bourguiba, Noura; Zid, Mohamed Faouzi; Driss, Ahmed

    2013-01-01

    The structure of the title compound tris­odium aluminium bis­(arsenate), Na3Al(AsO4)2, is built up from AlO4 and AsO4 corner-sharing tetra­hedra, forming an undulating two-dimensional framework parallel to (100). The layers are constituted of large Al6As6O36 rings made up from six AlO4 and AsO4 tetra­hedra in which two sodium cations are situated, the third sodium cation being located in the inter­layer space. The structural relationships between the title compound and Na3Fe(PO4)2, NaAlCo(PO4)2 and Al5Co3(PO4)8 are discussed. PMID:23424394

  20. 1,2,3,3',4',6'-Hexaacetyl-4,6-O-benzyl-idenesucrose.

    PubMed

    Brito-Arias, Marco A; Soto-Ortega, Miguel; García-Báez, Efrén V

    2011-01-26

    In the title compound, C(31)H(38)O(17), the 1,3-dioxane and pyran-oside rings both show (4)C(1) chair conformations while for the d-fructofuran-oside moiety an envelop 3E conformation is observed. The phenyl ring is oriented almost perpendicular to the 1,3-dioxane ring [dihedral angle = 79.3 (2)°], and the acetate groups are equatorial for the pyran-oside ring and axial for the furan-oside ring. The analysis of potential hydrogen bonds shows both intra- and inter-molecular C-H⋯O contacts to be present.

  1. 3-Methyl-1,2,4-triazolo[3,4-a]phthalazine monohydrate.

    PubMed

    Dutkiewicz, Grzegorz; Chidan Kumar, C S; Yathirajan, H S; Mayekar, A N; Kubicki, Maciej

    2009-10-10

    In the crystal structure of the title compound, C(10)H(8)N(4)·H(2)O, the organic mol-ecules are approximately planar [maximum deviation from the least-squares plane = 0.041 (2) Å]. Two mol-ecules are connected by two water mol-ecules via O-H⋯N hydrogen bonding into dimers, which are located around centres of inversion. In the crystal, mol-ecules are stacked in the a-axis direction, with mean distances between the π systems of 3.43 (1) and 3.46 (1) Å [centroid-centroid distances are 3.604 (2) and 3.591 (2) Å].

  2. 21 CFR 73.3122 - 4-[(2,4-dimethylphenyl)azo]-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-one.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 1 2013-04-01 2013-04-01 false 4- -2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-one. 73.3122 Section 73.3122 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN... exceed the minimum reasonably required to accomplish the intended coloring effect. (2) Authorization...

  3. 21 CFR 73.3122 - 4-[(2,4-dimethylphenyl)azo]-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-one.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 1 2012-04-01 2012-04-01 false 4- -2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-one. 73.3122 Section 73.3122 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN... exceed the minimum reasonably required to accomplish the intended coloring effect. (2) Authorization...

  4. AM2 3-4 Alternate Lay Pattern Evaluation

    DTIC Science & Technology

    2014-09-01

    ER D C/ G SL T R- 14 -3 8 Airfield Damage Repair Modernization Program AM2 3-4 Alternate Lay Pattern Evaluation G eo te ch ni ca l a nd...Airfield Damage Repair Modernization Program ERDC/GSL TR-14-38 September 2014 AM2 3-4 Alternate Lay Pattern Evaluation Timothy W. Rushing, Lyan...brickwork pattern. Therefore, the 3-4 alternate lay pattern was designed to allow Marines to use any mats on hand to fill in designated portions of the

  5. Dieth­yl(μ3-2-methyl-4-oxo-4H-pyran-3-olato-κ4 O 3,O 4:O 3:O 3)tris­(μ2-2-methyl-4-oxo-4H-pyran-3-olato-κ3 O 3,O 4:O 3)trizinc toluene disolvate

    PubMed Central

    Petrus, Rafał; Petrus, Joanna; Paszek, Karolina; Sobota, Piotr

    2013-01-01

    The title compound, [Zn3(C2H5)2(C6H5O3)42C7H8, crystallizes with one complex mol­ecule solvated by two mol­ecules of toluene in the asymmetric unit. The ZnII ions are coordinated by two terminal ethyl (Et) groups and four maltolate ligands, which act as μ3- and μ2-bridges. The metal atoms are arranged in an incomplete cubane Zn3O4 core structure, derived from one EtZnO3 tetra­hedron, one EtZnO4 bipyramid and one ZnO6 octa­hedron, sharing common corners. The structure is stabilized by weak C—H⋯O and C—H⋯π inter­actions. PMID:23723783

  6. 34. DETAILS OF CAISSON FOR PIERS 2, 3, 4 AND ...

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

    34. DETAILS OF CAISSON FOR PIERS 2, 3, 4 AND 5 TO BE BUILT ON SOIL OVERBURDEN - East Bloomsburg Bridge, Spanning Susquehanna River at Pennsylvania Route 487 (Legislative Route 283), Bloomsburg, Columbia County, PA

  7. 83. AGITATORS No. 2, No. 3, AND No. 4 FROM ...

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

    83. AGITATORS No. 2, No. 3, AND No. 4 FROM EAST. AIR SUPPLY RUNS THROUGH BENT BRACES ON RIGHT. NOTE AGITATOR RAKE LEANING AGAINST RETAINING WALL BETWEEN AGITATOR No. 2 AND No. 3. - Bald Mountain Gold Mill, Nevada Gulch at head of False Bottom Creek, Lead, Lawrence County, SD

  8. Platelet activating factor antagonist design. 2. X-ray structure of dimethyl 2,3,4,5-tetrahydro-5 beta-(3,4-methylenedioxyphenyl)-2-oxo-3 beta-(3,4,5-trimethoxybenzoyl)-3 alpha,4 alpha-furandicarboxylate.

    PubMed

    Peterson, J R; Do, H D; Rogers, R D

    1989-07-15

    C25H24O12, Mr = 516.46, triclinic, P-1, a = 8.780 (3), b = 11.298 (4), c = 13.271 (6) A, alpha = 71.77 (4), beta = 70.31 (3), gamma = 72.66 (3) degrees, V = 1189 A3, Z = 2, Dx = 1.44 g cm-3, lambda (Mo K alpha) = 0.71073 A, mu = 0.74 cm-1, F(000) = 540, T = 293 K, final R = 0.046 for 2495 observed [Fo greater than or equal to 5 sigma (Fo)] reflections. The observed structure reveals a trans disposition for the methoxycarbonyl and aryl substituents at positions 4 and 5 of the heterocycle and a cis-3,4-bis(methoxycarbonyl) relationship. There is no crystallographically imposed symmetry. Several intermolecular van der Waals interactions occur in the cell lattice of this compound.

  9. Method for preparation of 7-hydroxy-1,2,3,4-tetrahydroquinoline from 1,2,3,4-tetrahydroquinoline

    DOEpatents

    Field, George; Hammond, Peter R.

    1994-01-01

    Methods for the efficient preparation of 7-hydroxy-1,2,3,4-tetrahydroquinoline include a first method in which the acylation of m-aminophenol obtains a lactam which is reduced to give the desired quinoline and a second method in which tetrahydroquinoline is nitrated and hydrogenated and then hydrolyzed to obtain the desire quinoline. 7-hydroxy-1,2,3,4-tetrahydroquinoline is used in the efficient synthesis of four lasing dyes of the rhodamine class.

  10. Method for preparation of 7-hydroxy-1,2,3,4-tetrahydroquinoline from 1,2,3,4-tetrahydroquinoline

    DOEpatents

    Field, G.; Hammond, P.R.

    1994-02-01

    Methods for the efficient preparation of 7-hydroxy-1,2,3,4-tetrahydroquinoline include a first method in which the acylation of m-aminophenol obtains a lactam which is reduced to give the desired quinoline and a second method in which tetrahydroquinoline is nitrated and hydrogenated and then hydrolyzed to obtain the desire quinoline. 7-hydroxy-1,2,3,4-tetrahydroquinoline is used in the efficient synthesis of four lasing dyes of the rhodamine class.

  11. The absolute configuration of (2S,4S)- and (2R,4R)-2-tert-butyl-4-methyl-3-(4-tolylsulfonyl)-1,3-oxazolidine-4-carbaldehyde.

    PubMed

    Flock, Susanne; Bruhn, Clemens; Fink, Heinrich; Frauenrath, Herbert

    2006-02-01

    The title enantiomorphic compounds, C16H23NO4S, have been obtained in an enantiomerically pure form by crystallization from a diastereomeric mixture either of (2S,4S)- and (2R,4S)- or of (2R,4R)- and (2S,4R)-2-tert-butyl-4-methyl-3-(4-tolylsulfonyl)-1,3-oxazolidine-4-carbaldehyde. These mixtures were prepared by an aziridination rearrangement process starting with (S)- or (R)-2-tert-butyl-5-methyl-4H-1,3-dioxine. The crystal structures indicate an envelope conformation of the oxazolidine moiety for both compounds.

  12. Comparative study of the Mn4+2E → 4A2 luminescence in isostructural RE2Sn2O7:Mn4+ pyrochlores (RE3+ = Y3+, Lu3+ or Gd3+)

    NASA Astrophysics Data System (ADS)

    Senden, Tim; Broers, Fréderique T. H.; Meijerink, Andries

    2016-10-01

    Red emitting Mn4+-doped crystalline materials have potential for application in light emitting devices and therefore it is important to understand how the optical properties of Mn4+ are influenced by the host lattice the Mn4+ ions are situated in. In this work we investigate the effect of the host cations in the second coordination sphere on the Mn4+ emission by studying the luminescence of Mn4+ ions doped into three isostructural rare earth (RE) stannate RE2Sn2O7 pyrochlores (RE3+ = Y3+, Lu3+ or Gd3+). It is found that the energies of the Mn4+4T1 and 4T2 states significantly increase with decreasing Mn4+-O2- distance, whereas the energy of the 2E level shows a small shift to higher energies from RE3+ = Gd3+ to Lu3+ to Y3+. The observed trend for the 2E level energy is not related to the size of the RE3+ ion and is not in line with theoretical calculations reported previously. Low temperature emission spectra of the RE2Sn2O7:Mn4+ phosphors reveal that only asymmetrical vibronic modes couple to the 2E → 4A2 transition and furthermore show there is significant and unexpected local disorder for Mn4+ in Gd2Sn2O7 that is not observed for Mn4+ in the other hosts. Photoluminescence decay measurements demonstrate that the luminescence of RE2Sn2O7:Mn4+ is strongly quenched below room temperature which is assigned to non-radiative relaxation via a low-lying O2- → Mn4+ charge-transfer state.

  13. 10 CFR 960.3-2-2-4 - The environmental assessment.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 10 Energy 4 2011-01-01 2011-01-01 false The environmental assessment. 960.3-2-2-4 Section 960.3-2-2-4 Energy DEPARTMENT OF ENERGY GENERAL GUIDELINES FOR THE PRELIMINARY SCREENING OF POTENTIAL SITES FOR A NUCLEAR WASTE REPOSITORY Implementation Guidelines § 960.3-2-2-4 The environmental...

  14. 10 CFR 960.3-2-2-4 - The environmental assessment.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 10 Energy 4 2013-01-01 2013-01-01 false The environmental assessment. 960.3-2-2-4 Section 960.3-2-2-4 Energy DEPARTMENT OF ENERGY GENERAL GUIDELINES FOR THE PRELIMINARY SCREENING OF POTENTIAL SITES FOR A NUCLEAR WASTE REPOSITORY Implementation Guidelines § 960.3-2-2-4 The environmental...

  15. 10 CFR 960.3-2-2-4 - The environmental assessment.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 10 Energy 4 2012-01-01 2012-01-01 false The environmental assessment. 960.3-2-2-4 Section 960.3-2-2-4 Energy DEPARTMENT OF ENERGY GENERAL GUIDELINES FOR THE PRELIMINARY SCREENING OF POTENTIAL SITES FOR A NUCLEAR WASTE REPOSITORY Implementation Guidelines § 960.3-2-2-4 The environmental...

  16. 10 CFR 960.3-2-2-4 - The environmental assessment.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 10 Energy 4 2014-01-01 2014-01-01 false The environmental assessment. 960.3-2-2-4 Section 960.3-2-2-4 Energy DEPARTMENT OF ENERGY GENERAL GUIDELINES FOR THE PRELIMINARY SCREENING OF POTENTIAL SITES FOR A NUCLEAR WASTE REPOSITORY Implementation Guidelines § 960.3-2-2-4 The environmental...

  17. 10 CFR 960.3-2-2-4 - The environmental assessment.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 10 Energy 4 2010-01-01 2010-01-01 false The environmental assessment. 960.3-2-2-4 Section 960.3-2-2-4 Energy DEPARTMENT OF ENERGY GENERAL GUIDELINES FOR THE PRELIMINARY SCREENING OF POTENTIAL SITES FOR A NUCLEAR WASTE REPOSITORY Implementation Guidelines § 960.3-2-2-4 The environmental...

  18. 13. PRATT STREET BULKHEAD: SECTIONS 2, 3, 4, 5, AND ...

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

    13. PRATT STREET BULKHEAD: SECTIONS 2, 3, 4, 5, AND 6, DRAWER 10, PLAN NO. 1, 1 IN. = 15 FT. AND 1/2 IN. = 1 FT., APRIL 25, 1906, DRAWING SHOWS DESIGN FOR PRATT STREET BULKHEAD BETWEEN PIERS - Baltimore Inner Harbor, Pier 5, South of Pratt Street between Market Place & Concord Street, Baltimore, Independent City, MD

  19. Indiana Reading List. [Levels 1, 2, 3, and 4].

    ERIC Educational Resources Information Center

    Indiana State Dept. of Education, Indianapolis.

    This reading list is designed as a companion piece to Indiana's Academic Standards in English/Language Arts and is organized on four levels: Level 1, Grades K-2; Level 2, Grades 3-5; Level 3, Grades 6-8; and Level 4, Grades 9-12. It contains titles and authors for approximately 800 works. The Level 1 Reading List contains these sections: fiction…

  20. 3,4-Dihydroxy-1,6-bis(4-methoxyphenyl)hexa-2,4-diene-1,6-dione, its 4-methylphenyl analogue, and a potassium salt of 2-hydroxy-4-(4-methoxyphenyl)-4-oxobut-2-enoic acid.

    PubMed

    Nye, Luke; Turnbull, Mark M; Wikaira, Jan L

    2013-11-01

    Reaction of 4-methoxyacetophenone with diethyl oxalate under basic conditions produced 3,4-dihydroxy-1,6-bis(4-methoxyphenyl)hexa-2,4-diene-1,6-dione, C20H18O6, (1). The molecules lie across a crystallographic inversion centre and intramolecular hydrogen bonding, similar to acetylacetone, is observed, confirming that the molecule is in the di-enol-dione tautomeric form. Additional O-H...O hydrogen bonds link the molecules into chains parallel to the b axis. The structure is compared with that of redetermined 4-methylphenyl compound 3,4-dihydroxy-1,6-bis(4-methylphenyl)hexa-2,4-diene-1,6-dione, C20H18O4, (2), which crystallizes in a similar fashion. The salt, catena-poly[[μ2-2-hydroxy-4-(4-methoxyphenyl)-4-oxobut-2-enoato-κ(3)O(1),O(2):O(4)][μ2-2-hydroxy-4-(4-methoxyphenyl)-4-oxobut-2-enoic acid-κ(2)O(1):O(4)]potassium], [K(C11H9O5)(C11H10O5)]n, (3), was isolated as a by-product of the synthesis of (1). The two organic species are linked by a strong hydrogen bond between the carboxylic acid and carboxylate groups. They are further stabilized and linked into a double-chain structure via the seven-coordinate potassium ion.

  1. Full stereochemical understanding in a new (2R,3R,4R)-4-hydroxyisoleucine synthesis.

    PubMed

    Rolland, M; Kassem, T; Rolland, V; Martinez, J

    2001-12-01

    We present the crystal and molecular structures of 2,3,6,7,8,8a-hexahydro-6,8-methano-7,7,8a-trimethyl-3-(1-methyl-2-oxopropylidene)-5H-1,4-benzoxazin-2-one, C16H21NO3, (III), and 2,3,6,7,8,8a-hexahydro-3-(2-hydroxy-1-methylpropyl)-6,8-methano-7,7,8a-trimethyl-5H-1,4-benzoxazin-2-one, C16H25NO3, (V). These compounds are two of the four key intermediates in our synthetic route to (2R,3R,4R)-4-hydroxyisoleucine. The two structures provide a full understanding of the stereochemistry in successive steps. This synthesis was based on a new optically pure chiral oxazinone auxiliary derived from (1R,2R,5R)-2-hydroxypinan-3-one.

  2. Organically templated uranium(IV) fluorooxalates with layer structures: (H4TREN)[U2F6(C2O4)3].4H2O (TREN = tris(2-aminoethyl)amine) and (H4APPIP)[U2F6(C2O4)3].4H2O (APPIP = 1,4-bis(3-amino-propyl)piperazine).

    PubMed

    Wang, Chih-Min; Wu, Yi-Ying; Chen, Pei-Lin; Lii, Kwang-Hwa

    2007-03-14

    Two organically-templated layered uranium(IV) fluorooxalates, (H(4)TREN)[U(2)F(6)(C(2)O(4))(3)].4H(2)O (1) (TREN = tris(2-aminoethyl)amine) and (H(4)APPIP)[U(2)F(6)(C(2)O(4))(3)].4H(2)O (2) (APPIP = 1,4-bis(3-aminopropyl)piperazine), have been synthesized by hydrothermal methods and structurally characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and magnetic susceptibility. Both structures consist of anionic [U(2)F(6)(C(2)O(4))(3)](4-) layers separated by organic ammonium cations and lattice water molecules. The UF(3)O(6) polyhedra are connected by oxalate ligands in different ways within the layers. They are the first examples of organically-templated uranium fluorooxalates. Crystal data for compound 1 follow: monoclinic, P2(1)/c (No. 14), a = 19.1563(5) A, b = 8.9531(2) A, c = 16.6221(4) A, beta = 114.633(1) degrees, and Z = 4. Crystal data for compound are the same as those for 1 except a = 10.3309(8) A, b = 15.564(1) A, c = 17.537(1) A, and beta = 95.430(4) degrees.

  3. Anxiety Self Report (ASR (1,2,3,4,). X

    ERIC Educational Resources Information Center

    Parsons, Jane S.

    The Anxiety Self Report (ASR 1,2,3,4) is provided, followed by information about the report. The ASR is discussed as to its development, description, response bias, scoring procedures, reliability, stability, validity, and correlation between the ASR and the Manifest Anxiety Scale. (For related documents, see TM 002 928, 929.) (DB)

  4. A Reappraisal of the 4/3/2 Activity

    ERIC Educational Resources Information Center

    Boers, Frank

    2014-01-01

    In the 4/3/2 activity learners deliver the same talk three times under increasing time pressure. The activity is intended first and foremost to foster fluency, but accuracy and complexity have also been said to benefit from this activity. The present study investigates whether immediate repetition of monologues under increasing time pressure…

  5. 4-Methyl-3-(2-phenoxy­acet­yl)-5-phenyl-1,3,4-oxadiazinan-2-one

    PubMed Central

    Zukerman-Schpector, Julio; Sousa Madureira, Lucas; Rodrigues, Alessandro; Vinhato, Elisângela; Olivato, Paulo R.

    2009-01-01

    The 1,3,4-oxadiazinane ring in the title compound, C18H18N2O4, is in a twisted boat conformation. The two carbonyl groups are orientated towards the same side of the mol­ecule. The dihedral angle between the planes of the benzene rings is 76.6 (3)°. Mol­ecules are sustained in the three-dimensional structure by a combination of C—H⋯O, C—H⋯π and π–π [shortest centroid–centroid distance = 3.672 (6) Å] inter­actions. PMID:21582771

  6. (S)-Methyl 2-[(3R,4R)-2-benzyl-3-(2-fur-yl)-1-oxo-1,2,3,4-tetra-hydro-isoquinoline-4-carboxamido]-3-(1H-indol-3-yl)propanoate.

    PubMed

    Baktır, Zeliha; Akkurt, Mehmet; Kandinska, Meglena I; Bogdanov, Milen G; Büyükgüngör, Orhan

    2009-06-06

    The title compound, C(33)H(29)N(3)O(5), was synthesized by the reaction of racemic trans-2-benzyl-3-(2-fur-yl)-1-oxo-1,2,3,4-tetra-hydro-isoquinoline-4-carboxylic acid, l-tryptophan methyl ester and diisopropylcarbodiimide in dry dichloro-methane. The furan ring is disordered over two positions in a 0.859 (14):0.141 (14) ratio. In the 1,2,3,4-tetra-hydro-iso-quin-oline ring system, the heterocyclic ring is not planar, with puckering parameters Q(T) = 0.448 (2) Å, θ = 64.9 (3) and ϕ = 268.3 (3)°. The crystal is extended into a three-dimensional supra-molecular architecture through inter-molecular N-H⋯O hydrogen bonds and C-H⋯π inter-actions. The absolute structure was assigned by reference to the chiral starting material.

  7. Persistent luminescence properties of SrMg2(PO4)2:Eu2+,Tb3+

    NASA Astrophysics Data System (ADS)

    Ju, Guifang; Hu, Yihua; Chen, Li; Wang, Xiaojuan; Hung, Lihua

    2014-03-01

    We investigate the persistent luminescence in europium-doped SrMg2(PO4)2 upon codoping with auxiliary terbium. Luminescence properties of the phosphors, including photoluminescence, luminescence decay and thermoluminescence, are systematically studied. SrMg2(PO4)2:Eu2+ shows only a weak persistent luminescence, and codoping with Tb3+ is necessary to obtain considerable persistent luminescence. An energy level scheme is constructed to convey reasonable trapping and detrapping processes in the material.

  8. The system K2Mg2(SO4)3 (langbeinite)-K2Ca2(SO4)3 (calcium-langbeinite)

    USGS Publications Warehouse

    Morey, G.W.; Rowe, J.J.; Fournier, R.O.

    1964-01-01

    The join between the compositions K2Mg2(SO4)3 and K2Ca2(SO4)3 was studied by means of high-temperature equilibrium quenching techniques and by means of a heating stage mounted on an X-ray diffractometer. Complete solid solution exists in the system, but at 25??C members of the solid solution series are isometric only in the composition range 0-73??5 wt. per cent K2Ca2(SO4)3. At compositions richer in K2Ca2(SO4)3 than 73??5 wt. per cent, members of the series are optically biaxial. At higher temperatures members of the solid solution series are isometric at successively more calcium-rich compositions and pure K2Ca2(SO4)3 is isometric above about 200 ?? 2??C. The system is not binary, as mixtures richer in K2Ca2(SO4)3 than 42 wt. per cent decompose with the formation of liquid and CaSO4. ?? 1964.

  9. The 2.9-4.2 micron spectrum of Saturn: Clouds and CH 4, PH 3, and NH 3

    NASA Astrophysics Data System (ADS)

    Kim, Sang J.; Geballe, T. R.

    2005-12-01

    We have used synthetic spectra to analyze a medium resolution 2.9-4.2 μm spectrum of Saturn's temperate region observed at UKIRT using CGS4. The synthetic spectra include CH 4, PH 3, and NH 3 lines, for which mixing ratios were adopted from recent Cassini results. The observed absorption features in the spectrum are well accounted for by lines of these molecular species formed 22 +/- 8 km above the 1 bar pressure level at ˜610 mbar. The influence of optically thin haze particles at higher altitudes on the spectrum is not pronounced, with higher spectral resolution probably required to constrain the effects of haze in this wavelength region. Fluorescent line emission by CH 4 in its ν and ν+ν-ν bands, detected in the 3.2-3.5 μm region, originates between 400 km (˜0.06 mbar) and 800 km (˜0.01 μbar) above the 1 bar level, with peak contributions from the two major contributing bands at 550 km (˜3 μbar) and 700 km (˜0.1 μbar), respectively.

  10. Neutron diffraction studies of the Na-ion battery electrode materials NaCoCr2(PO4)3, NaNiCr2(PO4)3, and Na2Ni2Cr(PO4)3

    NASA Astrophysics Data System (ADS)

    Yahia, H. Ben; Essehli, R.; Avdeev, M.; Park, J.-B.; Sun, Y.-K.; Al-Maadeed, M. A.; Belharouak, I.

    2016-06-01

    The new compounds NaCoCr2(PO4)3, NaNiCr2(PO4)3, and Na2Ni2Cr(PO4)3 were synthesized by sol-gel method and their crystal structures were determined by using neutron powder diffraction data. These compounds were characterized by galvanometric cycling and cyclic voltammetry. NaCoCr2(PO4)3, NaNiCr2(PO4)3, and Na2Ni2Cr(PO4)3 crystallize with a stuffed α-CrPO4-type structure. The structure consists of a 3D-framework made of octahedra and tetrahedra that are sharing corners and/or edges generating channels along [100] and [010], in which the sodium atoms are located. Of significance, in the structures of NaNiCr2(PO4)3, and Na2Ni2Cr(PO4)3 a statistical disorder Ni2+/Cr3+ was observed on both the 8g and 4a atomic positions, whereas in NaCoCr2(PO4)3 the statistical disorder Co2+/Cr3+ was only observed on the 8g atomic position. When tested as negative electrode materials, NaCoCr2(PO4)3, NaNiCr2(PO4)3, and Na2Ni2Cr(PO4)3 delivered specific capacities of 352, 385, and 368 mA h g-1, respectively, which attests to the electrochemical activity of sodium in these compounds.

  11. Chiral pyridin-3-ones and pyridines: syntheses of enantiopure 2,4-disubstituted 6-hydroxy-1,6-dihydro-2H-pyridin-3-ones, 2,3-disubstituted 4-iodopyridines, and enantiopure 2,3-disubstituted 4-pyridinemethanols.

    PubMed

    Husain, Irfan; Saquib, Mohammad; Bajpai, Vikas; Kumar, Brijesh; Shaw, Arun K

    2011-11-04

    The development of an innovative method to access enantiopure 2,4-disubstituted 6-hydroxy-1,6-dihydro-2H-pyridin-3-ones starting from D-glucal via the aza-Achmatowicz transformation has been described. These highly functionalized pyridin-3-ones have been utilized for the synthesis of contiguously substituted pyridines through a rapid and efficient Et(3)N/Ac(2)O promoted cyclo-elimination, aromatization cascade, allowing the facile assembly of important pyridine-based building blocks like 2-substituted 3-acetoxy-4-iodopyridines and enantiopure 2-substituted 3-acetoxy-4-pyridinemethanols possessing benzylic stereogenic centers, whose synthesis otherwise would be tedious. The utilization of commercially available sugars as starting materials, mild reaction conditions, catalytic transfer hydrogen (CTH) of α-furfuryl azide derivatives, transfer of chiral aryl/alkyl methanols from enulosides to pyridin-3-ones and pyridines, high yields, and short reaction times are key features of this method. The utility of the method has been further exemplified by demonstrating the usage of the 2-substituted 3-acetoxy-4-iodopyridine for the construction of biologically significant molecules like 2,7-disubstituted furo[2,3-c]pyridines and 7,7'-disubstituted 2,2'-bifuro[2,3-c]pyridines.

  12. GC-MS and GC-IRD analysis of 2-, 3- and 4-methylmethamphetamine and 2-, 3- and 4-methylamphetamine.

    PubMed

    Davis, Sean; Blakey, Karen; Rands-Trevor, Karen

    2012-07-10

    4-Methylmethamphetamine has been detected in samples submitted for analysis in several states throughout Australia. Six ring substituted methyl isomers of methamphetamine and amphetamine were synthesised and analysed. As the regioisomeric 2-, 3- and 4-methylmethamphetamine and 2-, 3- and 4-methylamphetamine have virtually identical mass spectra, the use of MS is an ineffective technique to discriminate between these closely related compounds. We set out to determine whether the regioisomers could be differentiated by a combination of GC-MS, acetyl derivatisation and GC-IRD. We demonstrate that the three isomers of methylmethamphetamine and methylamphetamine can be separated by GC, and a combination of acetyl derivatisation and vapour phase IR can identify the specific ring substituted compound.

  13. 29 CFR 4.154 - Employees covered by sections 2(a)(3) and (4).

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 29 Labor 1 2010-07-01 2010-07-01 true Employees covered by sections 2(a)(3) and (4). 4.154 Section 4.154 Labor Office of the Secretary of Labor LABOR STANDARDS FOR FEDERAL SERVICE CONTRACTS Application of the McNamara-O'Hara Service Contract Act Employees Covered by the Act § 4.154 Employees...

  14. 3,6-Bis(2-pyridyl)di-1,2,4-triazolo[3,4-a:4',3'-c]phthalazine.

    PubMed

    Chang, Wen-Fu; Wen, Yuh-Sheng; Liu, Ling-Kang

    2004-09-01

    The title compound, C20H12N8, (I), has been prepared by the reaction of 1,4-dihydrazinophthalazine and pyridine-2-carboxaldehyde, followed by an oxidative cyclization by treatment with bromine. In the solid state, the molecules of (I) are discrete, comprising a fused and twisted four-ring system with an overall helical appearance. The distance between the two intramolecular pyridyl N atoms is 3.075 (2) A, this short contact distance suggesting a pi-pi interaction.

  15. Molecular and electronic structure of Re2Br4(PMe3)4

    DOE PAGES

    Johnstone, Erik V.; Poineau, Frederic; Todorova, Tanya K.; ...

    2016-07-07

    The dinuclear rhenium(II) complex Re2Br4(PMe3)4 was prepared from the reduction of [Re2Br8]2– with (n-Bu4N)BH4 in the presence of PMe3 in propanol. The complex was characterized by single-crystal X-ray diffraction (SCXRD) and UV–visible spectroscopy. It crystallizes in the monoclinic C2/c space group and is isostructural with its molybdenum and technetium analogues. The Re–Re distance (2.2521(3) Å) is slightly longer than the one in Re2Cl4(PMe3)4 (2.247(1) Å). The molecular and electronic structure of Re2X4(PMe3)4 (X = Cl, Br) were studied by multiconfigurational quantum chemical methods. The computed ground-state geometry is in excellent agreement with the experimental structure determined by SCXRD. The calculatedmore » total bond order (2.75) is consistent with the presence of an electron-rich triple bond and is similar to the one found for Re2Cl4(PMe3)4. The electronic absorption spectrum of Re2Br4(PMe3)4 was recorded in benzene and shows a series of low-intensity bands in the range 10 000–26 000 cm–1. The absorption bands were assigned based on calculations of the excitation energies with the multireference wave functions followed by second-order perturbation theory using the CASSCF/CASPT2 method. As a result, calculations predict that the lowest energy band corresponds to the δ* → σ* transition, while the next higher energy bands were attributed to the δ* → π*, δ → σ*, and δ → π* transitions.« less

  16. Fe2O3/Co3O4 composite nanoparticle ethanol sensor

    NASA Astrophysics Data System (ADS)

    Mirzaei, Ali; Park, Sunghoon; Sun, Gun-Joo; Kheel, Hyejoon; Lee, Chongmu; Lee, Sangmin

    2016-08-01

    In this study Fe2O3/Co3O4 nanocomposites were synthesized by using a simple hydrothermal route. The X-ray diffraction analysis results showed that the synthesized powders were pure and nanocrystalline in nature. Moreover, scanning electron microscopy revealed that Fe2O3 nanoparticles had spherical shapes while Co3O4 particles had a rod-like morphology. The ethanol sensing properties of Fe2O3/Co3O4 nanocomposites were examined and compared with those of pristine Fe2O3 nanoparticles. The gas sensing properties of Fe2O3/Co3O4 nanocomposites were shown to be superior to those of pristine Fe2O3 nanoparticles and for all concentrations of ethanol, the response of the nanocomposite sensor was shown to be higher than that of the pristine Fe2O3 nanoparticle sensor. In detail, the response of the Fe2O3/Co3O4 nanocomposite sensor to 200 ppm of ethanol at 300 °C was about 3 times higher than that of pristine sensor. Also, in general, the response and recovery times of the Fe2O3/Co3O4 nanocomposite sensor were shorter than those of the pristine one. The improved sensing characteristics of the Fe2O3/Co3O4 sensor were attributed to a combination of several effects: the formation of a potential barrier at the Fe2O3-Co3O4 interface, the enhanced modulation of the conduction channel width accompanying the adsorption and desorption of ethanol gas, the catalytic activity of Co3O4 for the oxidation of ethanol, the stronger oxygen adsorption of p-type Co3O4, and the formation of preferential adsorption sites.

  17. Spectral Analysis and Crystal Structures of 4-(4-Methylphenyl)-6-Phenyl-2,3,3a, 4-Tetrahydro-1H-Pyrido[3,2,1-jk]Carbazole and 4-(4-Methoxyphenyl)-6-Phenyl-2,3,3a, 4-Tetrahydro-1H-Pyrido[3,2,1-jk]Carbazole.

    PubMed

    Kalyana Sundar, J; Natarajan, S; Chitra, S; Paul, Nidhin; Manisankar, P; Muthusubramanian, S; Suresh, J

    2011-01-01

    The crystal structures of 4-(4-methylphenyl)-6-phenyl-2,3,3a,4-tetrahydro-1H-pyrido[3,2,1-jk]carbazole (IIa) and 4-(4-methoxyphenyl)-6-phenyl-2,3,3a,4-tetrahydro-1H-pyrido[3,2,1-jk]carbazole (IIb) were elucidated by single crystal X-ray diffraction. Compound (IIa), C28H25N, crystallizes in the triclinic system, space group P-1, with a = 8.936(2) Å, b = 10.490(1) Å, c = 11.801(1) Å, α = 102.69(5) (°) ,  β = 103.27(3) (°) , γ = 93.80(1) (°) , and Z = 2. The compound (IIb), C28H25NO, crystallizes in the monoclinic system, space group P21/a, with a = 11.376(5) Å, b = 14.139(3) Å, c = 13.237(4) Å, β = 97.41(3) (°) , and Z = 4. In both the structures, the pyrido ring adopts a twist boat conformation and the carbazole molecule has the twisted envelope structure with C3 and C13 at the flap. No classical hydrogen bonds are observed in the crystal structures. Details of the preparation, structures, and spectroscopic properties of the new compounds are discussed.

  18. (+/-)-4-Aryl-4,5-dihydro-3H-1,3-benzodiazepines. 2. Nuclear-substituted analogues of (+/-)-4,5-dihydro-2,3-dimethyl-4-phenyl-3H-1,3-benzodiazepine and (+/-)-4,5-dihydro-2-ethyl-3-methyl-4-phenyl-3H-1,3-benzodiazepine as potential antidepressant agents.

    PubMed

    Martin, L L; Setescak, L L; Worm, M; Crichlow, C A; Geyer, H M; Wilker, J C

    1982-04-01

    Antidepressant-like activity, as evidenced by marked inhibition of tetrabenazine-induced ptosis, was previously reported for (+/-)-4,5-dihydro-4-phenyl-3H-1,3-benzodiazepine derivatives. Since optimal antitetrabenazine activity was associated with (+/-)-4,5-dihydro-2,3-dimethyl-4-phenyl-3H-1,3-benzodiazepine (9k, HRP 543) and the 2-ethyl-3-methyl analogue (10k), the synthesis and evaluation of nuclear-substituted derivatives of these two compounds was also investigated. The initial synthesis involved Friedel-Crafts acylation of substituted benzenes with 2-nitrophenylacetyl chloride to afford 1-aryl-2-(2-nitrophenyl)ethanones 2, which were converted in five steps to (+/-)-alpha-aryl-N-methyl-2-nitrobenzeneethanamines 7. Greater flexibility with respect to the introduction of nuclear substituents was achieved by conversion of 2-nitrotoluene derivatives to 2 via acylation of intermediate beta-(dimethylamino)-2-nitrostyrenes with various aroyl chlorides and hydrolysis. Reductive amination of 2 with methylamine and sodium cyanoborohydride afforded 7 directly and significantly reduced the number of synthetic steps. Reduction of 7a-j to diamines 8a-j and cyclization with appropriate ortho esters gave nuclear-substituted analogues of 9k and 10k. Marked antitetrabenazine activity was associated with many of these compounds. Significant enhancement of activity with respect to the unsubstituted analogues 9k and 10k was not observed, with the exception of 9c which appeared to be slightly more potent than 9k.

  19. Diastereoselective synthesis of 2,3,4,5,6-pentafluoroheptanes.

    PubMed

    Farran, Daniel; Slawin, Alexandra M Z; Kirsch, Peer; O'Hagan, David

    2009-09-18

    A stereocontrolled synthesis of alkanes containing five contiguous fluorine atoms is presented. The compounds were prepared by sequential fluorination of diastereoisomeric alcohol-diepoxides. The chemistry involved epoxide ring-opening with HF.NEt(3) and deshydroxyfluorination reactions of free alcohols with Deoxo-Fluor. The fluorination reactions were all highly stereospecific, with all five fluorines being incorporated in three sequential steps. Three different diastereoisomers of the 2,3,4,5,6-pentafluoroheptyl motif were prepared as heptane-1,7-diol derivatives, a structural format amenable for incorporation of the vicinal pentafluoro scaffold into larger molecular architectures.

  20. Preparation of 1,1'-dinitro-3,3'-azo-1,2,4-triazole. [1,1'-dinitro-3,3'-azo-1,2,4-triazole

    DOEpatents

    Lee, K.Y.

    1985-03-05

    A new high density composition of matter, 1,1'-dinitro-3,3'-azo-1,2,4-triazole, has been synthesized using inexpensive, commonly available compounds. This compound has been found to be an explosive, and its use as a propellant is anticipated. 1 fig., 1 tab.

  1. 40 CFR 721.1637 - 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1-[2-[[(4...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1- oxy]ethoxy]-3-(2-propenyloxy)-4-methylbenzenesulfonate... Substances § 721.1637 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1-...

  2. 40 CFR 721.1637 - 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1-[2-[[(4...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 31 2011-07-01 2011-07-01 false 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1- oxy]ethoxy]-3-(2-propenyloxy)-4-methylbenzenesulfonate... Substances § 721.1637 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1-...

  3. 3-Amino-2-carbamoyl-4,6-diphenyl-4,5- and -4,7-dihydrothieno-(2,3-b)pyridines

    SciTech Connect

    Krauze, A.A.; Liepin'sh, E.E.; Dubur, G.Ya.

    1987-10-01

    The treatment of piperidinium salts of 3-cyano-1,4-dihydropyridine-2-thiols with alkyl halides leads to 2-alkylthio-3-cyano-1,4-dihydropyridines. The authors have shown that alkylation of the piperidinium salt of 4,6-diphenyl-3-cyano-1,4-dihydropyridine-2-thiol with iodoacetamide gives carbamoylmethylthio derivative II, which, by the action of an equimolar amount of a base with heating to 50-60/sup 0/C, gives a mixture of 3-amino-2-carbamoyl-4,6-diphenyl-4,7-dihydrothieno(2,3-b)pyridine and 3-amino-2-carbamoyl-4,6-diphenyl-4,5-dihydrothieno(2,3-b)-pyridine in a ratio of 1:1. In the presence of excess base the principal product is IV. It was established by PMR spectroscopy that dihydropyridine II initially undergoes cyclization to 4,7-dihydrothienopyridine III, which then undergoes isomerization to 4,5-dihydrothienopyridine IV. Acidification of a solution of IV in d/sub 6/-DMSO gives rise to reverse isomerization.

  4. (2E)-2-[2-(4-Chloro-phen-yl)hydrazin-1-yl-idene]-4,4,4-trifluoro-3-oxobutanal.

    PubMed

    Huo, Yan-Ping; Zhou, Li-Hua

    2010-06-16

    The title compound, C(10)H(6)ClF(3)N(2)O(2), was synthesized by coupling 4-dimethyl-amino-1,1,1-trifluoro-but-3-en-2-one with 4-chloro-benzene-diazo-nium chloride. It crystallizes with two mol-ecules in the asymmetric unit, which form two similar centrosymmetric dimers via hydrogen bonds. Extensive electron delocalization and intra-molecular N-H⋯O hydrogen bonds are responsible for a planar conformation of the mol-ecules (maximum deviations = 0.010 and -0.015 Å for the two molecules). In addition to hydrogen bonds, π-π stacking inter-actions with centroid-centroid distances of 3.604 (2) and 3.583 (2) Å contribute to the stability of the crystal structure.

  5. 3-Benzyl-7-(2,4-dichloro­phen­yl)-4H-1,3,4-thia­diazolo[2,3-c][1,2,4]triazin-4-one

    PubMed Central

    Fun, Hoong-Kun; Arshad, Suhana; Sarojini, B. K.; Imran, U. A.; Krishna, B.G.

    2012-01-01

    In the title compound, C17H10Cl2N4OS, the phenyl ring and the H atoms attached to the adjacent C atom are disordered over two positions, with refined site occupancies of 0.509 (8) and 0.491 (8). The planar 4H-1,3,4-thia­diazolo[2,3-c][1,2,4]triazine ring system [maximum deviation = 0.048 (3) Å] forms dihedral angles of 76.9 (5), 74.9 (5) and 9.88 (12)°, respectively, with the major and minor parts of the disordered phenyl ring and with the dichloro-substituted benzene ring. In the crystal, pairs of C—H⋯O hydrogen bonds link the mol­ecules, forming inversion dimers with an R 2 2(18) graph-set motif. A short S⋯N contact of 2.801 (3) Å is observed between the dimers. PMID:22719523

  6. 40 CFR 721.1637 - 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1-[2-[[(4...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 32 2012-07-01 2012-07-01 false 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1- oxy]ethoxy]-3-(2-propenyloxy)-4-methylbenzenesulfonate; and 2-propanol, 1- oxy] ethoxy]ethoxy]-3-(2-propenyloxy)-, 4-methylbenzenesulfonate. 721.1637 Section 721.1637 Protection of...

  7. From hydrated Ni3(OH)2(C8H4O4)2(H2O)4 to anhydrous Ni2(OH)2(C8H4O4): impact of structural transformations on magnetic properties.

    PubMed

    Mesbah, Adel; Rabu, Pierre; Sibille, Romain; Lebègue, Sébastien; Mazet, Thomas; Malaman, Bernard; François, Michel

    2014-01-21

    Dehydration of the hybrid compound [Ni3(OH)2(tp)2(H2O)4] (1) upon heating led to the sequential removal of coordinated water molecules to give [Ni3(OH)2(tp)2(H2O)2] (2) at T1 = 433 K and thereafter anhydrous [Ni2(OH)2(tp)] (3) at T2 = 483 K. These two successive structural transformations were thoroughly characterized by powder X-ray diffraction assisted by density functional theory calculations. The crystal structures of the two new compounds 2 and 3 were determined. It was shown that at T1 (433 K) the infinite nickel oxide chains built of the repeating structural unit [Ni33-OH)2](4+) in 1 collapse and lead to infinite porous layers, forming compound 2. The second transformation at T2 (483 K) gave the expected anhydrous compound 3, which is isostructural with Co2(OH)2(tp). These irreversible transitions directly affect the magnetic behavior of each phase. Hence, 1 was found to be antiferromagnetic at TN = 4.11 K, with metamagnetic behavior with a threshold field Hc of ca. 0.6 T. Compound 2 exhibits canted antiferromagnetism below TN = 3.19 K, and 3 is ferromagnetic below TC = 4.5 K.

  8. Propellant Containing 3, 6bis(1h-1,2,3,4-Tetrazol-5-Ylamino)-1,2,4,5- Tetrazine Or Salt Thereof

    DOEpatents

    Hiskey, Michael A.; Chavez, David E.; Naud, Darren

    2003-12-02

    The compound 3,6-bis(1H-1,2,3,4-tetrazol-5-ylamino)-1,2,4,5-tetrazine and its salts are provided together with a propellant composition including an oxidizer, a binder and 3,6-bis(1H-1,2,3,4-tetrazol-5-ylamino)-1,2,4,5-tetrazine or its salts.

  9. Discovery of N-(4-(2-Amino-3-chloropyridin-4-yloxy)-3-fluorophenyl)-4-ethoxy-1-(4-fluorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide (BMS-777607), a Selective and Orally Efficacious Inhibitor of the Met Kinase Superfamily

    SciTech Connect

    Schroeder, Gretchen M.; An, Yongmi; Cai, Zhen-Wei; Chen, Xiao-Tao; Clark, Cheryl; Cornelius, Lyndon A.M.; Dai, Jun; Gullo-Brown, Johnni; Gupta, Ashok; Henley, Benjamin; Hunt, John T.; Jeyaseelan, Robert; Kamath, Amrita; Kim, Kyoung; Lippy, Jonathan; Lombardo, Louis J.; Manne, Veeraswamy; Oppenheimer, Simone; Sack, John S.; Schmidt, Robert J.; Shen, Guoxiang; Stefanski, Kevin; Tokarski, John S.; Trainor, George L.; Wautlet, Barri S.; Wei, Donna; Williams, David K.; Zhang, Yingru; Zhang, Yueping; Fargnoli, Joseph; Borzilleri, Robert M.

    2009-12-01

    Substituted N-(4-(2-aminopyridin-4-yloxy)-3-fluoro-phenyl)-1-(4-fluorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamides were identified as potent and selective Met kinase inhibitors. Substitution of the pyridine 3-position gave improved enzyme potency, while substitution of the pyridone 4-position led to improved aqueous solubility and kinase selectivity. Analogue 10 demonstrated complete tumor stasis in a Met-dependent GTL-16 human gastric carcinoma xenograft model following oral administration. Because of its excellent in vivo efficacy and favorable pharmacokinetic and preclinical safety profiles, 10 has been advanced into phase I clinical trials.

  10. Oscillation in the Kmno 4NH 2CH 2COOHH 3PO 4 Cstr system

    NASA Astrophysics Data System (ADS)

    Li, Hexing; Huang, Xiaojun; Deng, Jingfa

    1996-08-01

    A novel chemical oscillating reaction in the KMnO 4NH 2CH 2COOHH 3PO 4 CSTR system in the presence and absence of Ag + has been described. The reaction kinetics in a closed Mn0 4-NH 2CH 2COOHH 3PO 4 system has been analyzed and a possible mechanism has been proposed. The catalytic effect of Ag + in the above reaction has also been studied.

  11. 3,4-trans-4-Aryl-3-(1-pyridinio)-1,2,3,4-tetrahydropyridine-6-thiolates--new group of potential cardiotonic drugs.

    PubMed

    Krauze, A; Vītoliņa, R; Garaliene, V; Sīle, L; Klusa, V; Duburs, G

    2005-11-01

    3,4-trans-4-Aryl-3-(1-pyridinio)-1,2,3,4-tetrahydropyridine-6-thiolates 6-11 were prepared by a Michael reaction of N-acetonylpyridinium chloride with 3-aryl-2-cyanothioacrylamides or by a one-pot three-carbon condensation of N-acetonylpyridinium chloride, aromatic aldehyde and 2-cyanothioacetamide, and their cardiotonic properties were studied. 3,4-trans-5-cyano-2-hydroxy-2-methyl-4-(3-nitrophenyl)-3-(1-pyridinio)-1,2,3,4-tetrahydropyridine-6-thiolate 8 was considered as a lead compound in this series since it in vitro experiments (spontaneously beating rat atria) showed a cardiotonic activity similar to that of milrinone 2, however compound 8 induced activity at lover concentrations and without influence on chronotropic action of the heart. Unlike milrinone 2, thiolate 8 in vivo experiments (anaesthetized rats) did not influence blood pressure and heart rate. The acute toxicity of compound 8 was more than 10 times lower than that of milrinone 2.

  12. Enantioselective one-pot synthesis of 2-amino-4-(indol-3-yl)-4H-chromenes.

    PubMed

    Chen, Weiliang; Cai, Yunfei; Fu, Xuan; Liu, Xiaohua; Lin, Lili; Feng, Xiaoming

    2011-09-16

    An enantioselective one-pot synthesis of 2-amino-4-(indol-3-yl)-4H-chromenes via a Knoevenagel/Pinner/Friedel-Crafts reaction of salicylaldehyde, malononitrile, and indole is presented. Moderate to good yields (up to 89%) and high enantioselectivities (up to 90% ee) were obtained with an N,N'-dioxide-Zn(II) complex as the catalyst. This strategy provides an efficient and convenient method to access enantiomerically enriched 2-amino-4H-chromene derivatives.

  13. 40 CFR 721.1637 - 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1-[2-[[(4...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 32 2013-07-01 2013-07-01 false 1,2-Propanediol, 3-(2-propenyloxy... Substances § 721.1637 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1- oxy.... (1) The chemical substances 1,2-propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzenesulfonate) (PMN...

  14. 40 CFR 721.1637 - 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1-[2-[[(4...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false 1,2-Propanediol, 3-(2-propenyloxy... Substances § 721.1637 1,2-Propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzene sulfonate); 2-propanol, 1- oxy.... (1) The chemical substances 1,2-propanediol, 3-(2-propenyloxy)-, bis(4-methylbenzenesulfonate) (PMN...

  15. Effect of Sr doping in layered Eu3Bi2S4F4 superconductor

    NASA Astrophysics Data System (ADS)

    Zhang, Pan; Zhai, Hui-Fei; Wang, Zhen; Chen, Jian; Feng, Chun-Mu; Cao, Guang-Han; Xu, Zhu-An

    2017-01-01

    We report the effect of Sr-doping in the BiS2-based superconductor {{Eu}}3-xSr x Bi2S4F4. Eu3Bi2S4F4 is a self-doped compound with a mixed Eu valence state. By the partial substitution of Sr for Eu, T c gradually decreases and superconductivity disappears above 0.3 K when x\\gt 1.0. Magnetic-susceptibility and specific-heat measurements reveal that Sr substitution leads to a decrease in both Eu2+ and Eu3+ populations. The decreased Eu3+ population, and the corresponding lower charge carrier density, may be the main origin for the suppression of superconductivity. In addition, we find a significant increase in the Sommerfeld coefficient {γ }0 upon Sr doping, which may be due to the Kondo effect between the magnetic moments (associated to Eu2+ ions) and the conducting electrons. This work implies that the Kondo effect could compete with superconductivity in Eu3Bi2S4F4.

  16. Li 3V 2(PO 4) 3 cathode material synthesized by chemical reduction and lithiation method

    NASA Astrophysics Data System (ADS)

    Zheng, Jun-Chao; Li, Xin-Hai; Wang, Zhi-Xing; Guo, Hua-Jun; Hu, Qi-Yang; Peng, Wen-Jie

    The monoclinic-type Li 3V 2(PO 4) 3 cathode material was synthesized via calcining amorphous Li 3V 2(PO 4) 3 obtained by chemical reduction and lithiation of V 2O 5 using oxalic acid as reducer and lithium carbonate as lithium source in alcohol solution. The amorphous Li 3V 2(PO 4) 3 precursor was characterized by using TG-DSC and XPS. The results showed that the V 5+ was reduced to V 3+ by oxalic acid at ambient temperature and pressure. The prepared Li 3V 2(PO 4) 3 was characterized by XRD and SEM. The results indicated the Li 3V 2(PO 4) 3 powder had good crystallinity and mesoporous morphology with an average diameter of about 30 nm. The pure Li 3V 2(PO 4) 3 exhibits a stable discharge capacity of 130.08 mAh g -1 at 0.1 C (14 mA g -1).

  17. Thermodynamics of Cr2O3, FeCr2O4, ZnCr2O4 and CoCr2O4

    SciTech Connect

    Ziemniak SE, Anovitz LM, Castelli RA, Porter WD

    2007-01-09

    High temperature heat capacity measurements were obtained for Cr{sub 2}O{sub 3}, FeCr{sub 2}O{sub 4}, ZnCr{sub 2}O{sub 4} and CoCr{sub 2}O{sub 4} using a differential scanning calorimeter. These data were combined with previously-available, overlapping heat capacity data at temperatures up to 400 K and fitted to 5-parameter Maier-Kelley C{sub p}(T) equations. Expressions for molar entropy were then derived by suitable integration of the Maier-Kelley equations in combination with recent S{sup o}(298) evaluations. Finally, a database of high temperature equilibrium measurements on the formation of these oxides was constructed and critically evaluated. Gibbs energies of Cr{sub 2}O{sub 3}, FeCr{sub 2}O{sub 4} and CoCr{sub 2}O{sub 4} were referenced by averaging the most reliable results at reference temperatures of 1100, 1400 and 1373 K, respectively, while Gibbs energies for ZnCr{sub 2}O{sub 4} were referenced to the results of Jacob [Thermochim. Acta 15 (1976) 79-87] at 1100 K. Thermodynamic extrapolations from the high temperature reference points to 298.15 K by application of the heat capacity correlations gave {Delta}{sub f}G{sup o}(298) = -1049.96, -1339.40, -1428.35 and -1326.75 kJ mol{sup -1} for Cr{sub 2}O{sub 3}, FeCr{sub 2}O{sub 4}, ZnCr{sub 2}O{sub 4} and CoCr{sub 2}O{sub 4}, respectively.

  18. The microbial degradation of phenylalkanes. 2-Phenylbutane, 3-phenylpentane, 3-phenyldodecane and 4-phenylheptane

    PubMed Central

    Baggi, G.; Catelani, D.; Galli, E.; Treccani, V.

    1972-01-01

    1. Two Pseudomonas strains capable of utilizing 2-phenylbutane, 3-phenylpentane and 4-phenylheptane as the sole carbon and energy source were isolated. 2. Two Nocardia strains capable of utilizing only 3-phenyldodecane as the sole carbon and energy source were isolated. 3. All the isolated strains were unable to grow on the corresponding phenylalkane-p-sulphonates. 4. From liquid cultures of Pseudomonas strains utilizing 2-phenylbutane, 2-(2,3-dihydro-2,3-dihydroxyphenyl)butane was isolated and identified. Evidence for a meta cleavage of the benzene ring was also obtained. 5. From liquid cultures of Pseudomonas strains utilizing 3-phenylpentane, 3-(2,3-dihydro-2,3-dihydroxyphenyl)pentane and 2-hydroxy-7-ethyl-6-oxonona-2,4-dienoic acid were isolated and identified. 6. Evidence for the formation of both a diol and a meta-cleavage compound was obtained from liquid cultures of both Pseudomonas strains utilizing 4-phenylheptane. 7. Liquid cultures of both Nocardia strains utilizing 3-phenyldodecane never formed a diol or a semialdehyde-related compound. 2-Phenylbutyric acid, 3-phenylvaleric acid and 4-phenylhexanoic acid were shown to be present in these cultures. PMID:5073722

  19. [Zn3(PO4)2(H2O)(0.8)(NH3)(1.2)].

    PubMed

    Stojanović, Jovica; Dordević, Tamara; Karanović, Ljiljana

    2010-05-01

    The structure of the title compound, ammineaquadi-mu(5)-phosphato-trizinc(II), [Zn(3)(PO(4))(2)(H(2)O)(0.8)(NH(3))(1.2)], consists of two parts: (i) PO(4) and ZnO(4) vertex-sharing tetrahedra arranged in layers parallel to (100) and (ii) ZnO(2)(N/O)(2) tetrahedra located between the layers. Elemental analysis establishes the ammine-to-water ratio as 3:2. ZnO(2)(N/O)(2) tetrahedra are located at special position 4e (site symmetry 2) in C2/c. The two O atoms of ZnO(2)(N/O)(2) are bonded to neighbouring P atoms, forming two Zn-O-P linkages and connecting ZnO(2)(N/O)(2) tetrahedra with two adjacent bc plane layers. A noteworthy feature of the structure is the presence of NH(3) and H(2)O at the same crystallographic position and, consequently, qualitative changes in the pattern of hydrogen bonding and weaker N/O-H...O electrostatic interactions, as compared to two closely related structures.

  20. BPO4@B2O3 and (BPO4@B2O3):Eu3+: The novel single-emitting-component phosphors for near UV-white LEDs

    NASA Astrophysics Data System (ADS)

    Cao, Xiyu; Liu, Wei; Jiang, Yu; Cao, Lixin; Su, Ge; Gao, Rongjie

    2016-08-01

    Nowadays much effort has been devoted to exploring novel luminescent materials with low-cost, high stability and excellent luminescent properties. In this paper, a new kind of luminescent material BPO4@B2O3 was prepared by using a facile method. The as-obtained samples contain numerous BPO4 nanoparticles enclosed by amorphous and crystalline B2O3 homogeneously, which exhibits a broad emission band ranging from 380 to 700 nm under near-UV irradiation. More importantly, it is worth noting that the BPO4@B2O3 phosphor exhibits the excellent thermal quenching property, which endows it with a promising prospect as phosphors for high power white LEDs. To further promote its application as white light phosphors, Eu3+ ions were doped into the BPO4@B2O3 samples and prepared the (BPO4@B2O3):Eu3+ phosphors with chromaticity coordinates (0.3022, 0.3122). The corresponding packaging of LEDs indicates that both BPO4@B2O3 and (BPO4@B2O3):Eu3+ can be considered as the promising phosphors for WLEDs.

  1. Tellurium-bridged manganese carbonyl clusters: synthesis and structural transformations of [Te4Mn3(CO10]-, [Te2Mn3(CO)9]2-, [Te2Mn3(CO)9]-, and [Te2Mn4(CO)12]2-.

    PubMed

    Shieh, M; Chen, H S; Yang, H Y; Lin, S F; Ueng, C H

    2001-07-16

    The reactions of appropriate ratios of K2TeO3 and [Mn2(CO)10)] in superheated methanol solutions lead to a series of novel cluster anions [Te4Mn3(CO)10] (1), [Te2Mn3(CO)9]2- (2), [Te2Mn3(CO)9]- (3), and [Te2Mn4(CO)12]2- (4). When cluster 1 is treated with [Mn2(CO)10]/KOH in methanol, paramagnetic cluster 2 is formed in moderate yield. Cluster 2 is oxidized by [Cu(MeCN)4]BF4 to give the closo-cluster [Te2Mn3(CO)9]- (3), while treatment of 2 with [Mn2(CO)10]/KOH affords the closo-cluster 4. IR spectroscopy showed that cluster 1 reacted with [Mn2(CO)10] to give cluster 4 via cluster 2. Clusters 1-4 were structurally characterized by spectroscopic methods or/and X-ray analyses. The core structure of 1 can be described as two [Mn(CO)3] groups doubly bridged by two Te2 fragments in a mu2-eta2 fashion. Both [Mn(CO)3] groups are further coordinated to one [Mn(CO)4] moiety. Cluster 2 is a 49 e- species with a square-pyramidal core geometry. While cluster 3 displays a trigonal-bipyramidal metal core, cluster 4 possesses an octahedral core geometry.

  2. Synthesis and anticancer evaluation of 3-substituted quinolin-4-ones and 2,3-dihydroquinolin-4-ones.

    PubMed

    Rajput, Santosh; Gardner, Christopher R; Failes, Timothy W; Arndt, Greg M; Black, David Stc; Kumar, Naresh

    2014-01-01

    A series of 3-aryl-5,7-dimethoxyquinolin-4-ones 8 and 3-aryl-5,7-dimethoxy-2,3-dihydroquinolin-4-ones 13 were synthesized in good yields. Demethylation under a range of conditions afforded the corresponding 5-hydroxy and 5,7-dihydroxy derivatives. Biological evaluation against a range of cancer cells lines showed that the quinolin-4-one scaffold was more cytotoxic than the reduced 2,3-dihydroquinolin-4-one scaffold. The most active monohydroxy compound 15f demonstrated 85.9-99% reduction in cell viability against the cell lines tested.

  3. A Novel Monomeric Tin(II) Phosphate, [N(C 2H 5NH 3) 3] 3+[Sn(PO 4)(HPO 4)] 34H 2O, Connected through Hydrogen Bonding

    NASA Astrophysics Data System (ADS)

    Ayyappan, S.; Cheetham, A. K.; Natarajan, Srinivasan; Rao, C. N. R.

    1998-08-01

    The tin(II) phosphate, [N(C 2H 5NH 3) 3] 3+[Sn(PO 4)(HPO 4)] 3-4H 2O, contains monomeric Sn 2(PO 4) 2(HPO 4) 2units which form a hydrogen-bonded network with the TREN amine (TREN=N(C 2H 5NH 3) 3+3); triclinic, space group P1 (no. 2), a=9.579(1), b=10.507(1), c=10.976(1) Å; α=72.93(1)°, β=78.03(1)°, γ=69.82(1)°, V=984.2(1) Å 3, Z=2. The Sn 2P 2O 4core of this unit is a common structural feature of open-framework tin phosphates and may play a role as a building block for this class of materials.

  4. Photosynthesis of C3, C3–C4, and C4 grasses at glacial CO2

    PubMed Central

    Pinto, Harshini; Sharwood, Robert E.; Tissue, David T.; Ghannoum, Oula

    2014-01-01

    Most physiology comparisons of C3 and C4 plants are made under current or elevated concentrations of atmospheric CO2 which do not reflect the low CO2 environment under which C4 photosynthesis has evolved. Accordingly, photosynthetic nitrogen (PNUE) and water (PWUE) use efficiency, and the activity of the photosynthetic carboxylases [Rubisco and phosphoenolpyruvate carboxylase (PEPC)] and decarboxylases [NADP-malic enzyme (NADP-ME) and phosphoenolpyruvate carboxykinase (PEP-CK)] were compared in eight C4 grasses with NAD-ME, PCK, and NADP-ME subtypes, one C3 grass, and one C3–C4 grass grown under ambient (400 μl l–1) and glacial (180 μl l–1) CO2. Glacial CO2 caused a smaller reduction of photosynthesis and a greater increase of stomatal conductance in C4 relative to C3 and C3–C4 species. Panicum bisulcatum (C3) acclimated to glacial [CO2] by doubling Rubisco activity, while Rubisco was unchanged in Panicum milioides (C3–C4), possibly due to its high leaf N and Rubisco contents. Glacial CO2 up-regulated Rubisco and PEPC activities in concert for several C4 grasses, while NADP-ME and PEP-CK activities were unchanged, reflecting the high control exerted by the carboxylases relative to the decarboxylases on the efficiency of C4 metabolism. Despite having larger stomatal conductance at glacial CO2, C4 species maintained greater PWUE and PNUE relative to C3–C4 and C3 species due to higher photosynthetic rates. Relative to other C4 subtypes, NAD-ME and PEP-CK grasses had the highest PWUE and PNUE, respectively; relative to C3, the C3–C4 grass had higher PWUE and similar PNUE at glacial CO2. Biomass accumulation was reduced by glacial CO2 in the C3 grass relative to the C3–C4 grass, while biomass was less reduced in NAD-ME grasses compared with NADP-ME and PCK grasses. Under glacial CO2, high resource use efficiency offers a key evolutionary advantage for the transition from C3 to C4 photosynthesis in water- and nutrient-limited environments. PMID:24723409

  5. Synthesis and optical properties of ZnAl2O4:Cr3+, Tb3+ powders

    NASA Astrophysics Data System (ADS)

    Thi Loan, Trinh; Thi Thuy, Nguyen; Long, Nguyen Ngoc

    2013-10-01

    ZnAl2O4:Cr3+, Tb3+ powders with different dopant contents have been synthesized by sol-gel method using the following precursors: zinc nitrate (Zn(NO3)2), aluminum nitrate (Al(NO3)3), terbium nitrate (Tb(NO3)3), chrome nitrate (Cr(NO3)3), and citric acid. The effect of the Cr3+, Tb3+ concentration and heat-treating temperature on structural and optical properties of the synthesized samples has been studied. International Workshop on Advanced Materials and Nanotechnology 2012 (IWAMN 2012).

  6. 3-tert-Butyl 5-methyl (2R,4S,5R)-2-(4-methoxyphenyl)-4-(3-nitrophenyl)-1,3-oxazolidine-3,5-dicarboxylate

    PubMed Central

    Montiel-Smith, Sara; Bernès, Sylvain; Sandoval-Ramírez, Jesús; Meza-Reyes, Socorro; Dubois, Joëlle

    2012-01-01

    The title mol­ecule, C23H26N2O8, was synthesized in three steps starting from m-nitro­cinnamic acid. The central oxazolidine ring adopts an almost perfect envelope conformation with the O atom as the flap [puckering parameter ϕ = 0.3 (6)°]. The dihedral angle formed by the benzene rings is 61.81 (9)°. In the crystal, mol­ecules are connected into double chains parallel to [010] by C—H⋯O hydrogen bonds. The absolute configuration was assigned from the synthetic procedure. PMID:23284466

  7. Phosphine-Catalyzed Annulations of Azomethine Imines: Allene-Dependent [3 + 2], [3 + 3], [4 + 3], and [3 + 2 + 3] Pathways

    PubMed Central

    Na, Risong; Jing, Chengfeng; Xu, Qihai; Jiang, Hui; Wu, Xi; Shi, Jiayan; Zhong, Jiangchun; Wang, Min; Benitez, Diego; Tkatchouk, Ekaterina; Goddard, William A.; Guo, Hongchao; Kwon, Ohyun

    2011-01-01

    In this paper we describe the phosphine-catalyzed [3 + 2], [3 + 3], [4 + 3], and [3 + 2 + 3] annulations of azomethine imines and allenoates. These processes mark the first use of azomethine imines in nucleophilic phosphine catalysis, producing dinitrogen-fused heterocycles, including tetrahydropyrazolo-pyrazolones, -pyridazinones, -diazepinones, and -diazocinones. Counting the two different reaction modes in the [3 + 3] cyclizations, there are five distinct reaction pathways—the choice of which depends on the structure and chemical properties of the allenoate. All reactions are operationally simple and proceed smoothly under mild reaction conditions, affording a broad range of 1,2-dinitrogen–containing heterocycles in moderate to excellent yields. A zwitterionic intermediate formed from a phosphine and two molecules of ethyl 2,3-butadienoate acted as a 1,5-dipole in the annulations of azomethine imines, leading to the [3 + 2 + 3] tetrahydropyrazolodiazocinone products. The incorporation of two molecules of an allenoate into an eight-membered-ring product represents a new application of this versatile class of molecules in nucleophilic phosphine catalysis. The salient features of this protocol—the facile access to a diverse range of nitrogen-containing heterocycles and the simple preparation of azomethine imine substrates—suggest that it might find extensive applications in heterocycle synthesis. PMID:21812448

  8. Enhanced visible-light photocatalytic decomposition of 2,4-dichlorophenoxyacetic acid over ZnIn2S4/g-C3N4 photocatalyst.

    PubMed

    Qiu, Pengxiang; Yao, Jinhua; Chen, Huan; Jiang, Fang; Xie, Xianchuan

    2016-11-05

    ZnIn2S4/g-C3N4 heterojunction photocatalyst was successfully synthesized via a simple hydrothermal method and applied to visible-light photocatalytic decomposition of 2,4-dichlorophenoxyacetic acid (2,4-D) from aqueous phase. The flower-like ZnIn2S4 particles were dispersed on the surface of g-C3N4 nanosheets in the ZnIn2S4/g-C3N4 composite. The composite showed higher separation rate of electron-hole pairs as compared to ZnIn2S4 and g-C3N4. Consequently, the ZnIn2S4/g-C3N4 composite exhibited enhanced visible light photocatalytic decomposition efficiency of 2,4-D, within 20% ZnIn2S4/g-C3N4 composite owning the highest photocatalytic efficiency and initial rate. The initial rates of 2,4-D degradation on g-C3N4, ZnIn2S4, and 20% ZnIn2S4/g-C3N4 were 1.23, 0.57 and 3.69mmol/(gcath), respectively. The h(+) and O2(-) were found to be the dominant active species for 2,4-D decomposition. The photocatalytic degradation pathways of 2,4-D by ZnIn2S4/g-C3N4 under visible light irradiation were explored. The ZnIn2S4/g-C3N4 composite displayed high photostability in recycling tests, reflecting its promising potential as an effective visible light photocatalyst for 2,4-D treatment.

  9. Anomalous Eu valence state and superconductivity in undoped Eu3Bi2S4F4.

    PubMed

    Zhai, Hui-Fei; Zhang, Pan; Wu, Si-Qi; He, Chao-Yang; Tang, Zhang-Tu; Jiang, Hao; Sun, Yun-Lei; Bao, Jin-Ke; Nowik, Israel; Felner, Israel; Zeng, Yue-Wu; Li, Yu-Ke; Xu, Xiao-Feng; Tao, Qian; Xu, Zhu-An; Cao, Guang-Han

    2014-10-29

    We have synthesized a novel europium bismuth sulfofluoride, Eu3Bi2S4F4, by solid-state reactions in sealed evacuated quartz ampules. The compound crystallizes in a tetragonal lattice (space group I4/mmm, a = 4.0771(1) Å, c = 32.4330(6) Å, and Z = 2), in which CaF2-type Eu3F4 layers and NaCl-like BiS2 bilayers stack alternately along the crystallographic c axis. There are two crystallographically distinct Eu sites, Eu(1) and Eu(2) at the Wyckoff positions 4e and 2a, respectively. Our bond valence sum calculation, based on the refined structural data, indicates that Eu(1) is essentially divalent, while Eu(2) has an average valence of ∼ +2.64(5). This anomalous Eu valence state is further confirmed and supported, respectively, by Mössbauer and magnetization measurements. The Eu(3+) components donate electrons into the conduction bands that are mainly composed of Bi 6px and 6py states. Consequently, the material itself shows metallic conduction and superconducts at 1.5 K without extrinsic chemical doping.

  10. High pressure structural investigation on alluaudites Na2Fe3(PO4)3-Na2FeMn2(PO4)3 system

    NASA Astrophysics Data System (ADS)

    Gao, Jing; Huang, Weifeng; Qin, Shan; Wu, Xiang

    2017-03-01

    Alluaudites are promising electrochemical materials benefited from the open structure. Structural variations of alluaudites Na2M3(PO4)3 (M3=Fe3, Fe2Mn and FeMn2) system have been studied by synchrotron radiation X-ray diffraction combined with diamond anvil cell technique up to 10 GPa at room temperature. No phase transition is observed. The excellent structural stability is mainly due to the flexible framework plus strong covalent P-O bond. Mn2+ instead of Fe can be described as Na++2Fe2+→Mn2++Fe3++□ where □ represents a lattice vacancy. The replacement of Fe with larger Mn2+ is equivalent to applying negative chemical pressure to the material. And it causes a more compressible b-axis, lattice expansion, structural compressibility and intensifies the core/electron-electron interactions of Fe. External pressure effect produces anisotropic lattice shrinkage. Structural considerations related to these variations and promising application prospects are discussed.

  11. Metabolism of 1,2,3,4-, 1,2,3,5-, and 1,2,4,5-tetrachlorobenzene in the squirrel monkey

    SciTech Connect

    Schwartz, H.; Chu, I.; Villeneuve, D.C.; Benoit, F.M.

    1987-01-01

    The metabolism of three tetrachlorobenzene isomers (TeCB) was investigated in the squirrel monkey. The animals were administered orally 6 single doses of /sup 14/C-labeled 1,2,3,4-, 1,2,4,5-, or 1,2,3,5-tetrachlorobenzene over a 3-wk period at levels ranging from 50 to 100 mg/kg body weight (b.w) and kept in individual metabolism cages to collect urine and feces for radioassay. Approximately 38% (1,2,3,4-TeCB), 36% (1,2,3,5-TeCB), and 18% (1,2,4,5-TeCB) of the doses were excreted respectively in the feces 48 h post administration. In monkeys dosed with 1,2,3,4-TeCB, unchanged compound accounted for 50% of the fecal radioactivity. Unchanged compound accounted for more than 50% of the fecal radioactivity found in the monkeys dosed with 1,2,3,5-TeCB. The fecal metabolites were identified in both groups. No metabolites were detected in the feces of monkeys dosed with 1,2,4,5-TeCB. While the fecal route represented the major route of excretion for 1,2,3,4-TeCB, the other two isomers were eliminated exclusively in the feces. The above data in the squirrel monkey are different from those obtained with the rat and the rabbit, and demonstrate the different metabolic pathways for the isomers.

  12. Regioselective synthesis of novel 3-allyl-2-(substituted imino)-4-phenyl-3H-thiazole and 2,2‧-(1,3-phenylene)bis(3-substituted-2-imino-4-phenyl-3H-thiazole) derivatives as antibacterial agents

    NASA Astrophysics Data System (ADS)

    Abbasi Shiran, Jafar; Yahyazadeh, Asieh; Mamaghani, Manouchehr; Rassa, Mehdi

    2013-05-01

    Several novel 3-allyl-2-(substituted imino)-4-phenyl-3H-thiazole derivatives were synthesized by the reaction of allyl-thioureas and 2-bromoacetophenone. We also report the synthesis of bis-allyl-3H thiazoles using the reaction of various isothiocyanates and 1,3-phenylenediamine. The structures of all compounds were characterized by spectral and elemental analysis. Most of the synthesized compounds exhibited efficient antibacterial activities against Salmonella enterica, Micrococcus luteus, Bacillus subtilis and Pseudomonas aeruginosa.

  13. C4H2, HC3N and C2N2 in Titan's atmosphere

    NASA Astrophysics Data System (ADS)

    Kunde, V. G.; Aikin, A. C.; Hanel, R. A.; Jennings, D. E.; Maguire, W. C.; Samuelson, R. E.

    1981-08-01

    Voyager 1 took IR measurements of the atmosphere of Titan, and obtained an average of 346 spectra, mostly from the center of the disk. The compounds C4H2, HC3N, and C2N2 were detected in the atmosphere of Titan. The identification of two compounds containing nitrogen, in addition to HCN, provides further evidence for the abundance of free N2 on Titan. The organic compounds observed in the atmosphere of Titan are summarized in a table, which also indicates the approximate mole fraction for each compound identified previously. The observed compounds originate by reactions of methane and nitrogen radicals in a predominantly nitrogen atmosphere.

  14. Safety testing of AGR-2 UO2 compacts 3-3-2 and 3-4-2

    SciTech Connect

    Hunn, John D.; Morris, Robert Noel; Baldwin, Charles A.; Montgomery, Fred C.

    2015-09-01

    Post-irradiation examination (PIE) is in progress on tristructural-isotropic (TRISO) coated-particle fuel compacts from the Advanced Gas Reactor (AGR) Fuel Development and Qualification Program second irradiation experiment (AGR-2) [Collin 2014]. The AGR-2 PIE will build upon new information and understanding acquired throughout the recently-concluded six-year AGR-1 PIE campaign [Demkowicz et al. 2015] and establish a database for the different AGR-2 fuel designs.

  15. Lysyl oxidase-like 2 (LOXL2) oxidizes trimethylated lysine 4 in histone H3.

    PubMed

    Herranz, Nicolás; Dave, Natàlia; Millanes-Romero, Alba; Pascual-Reguant, Laura; Morey, Lluis; Díaz, Víctor M; Lórenz-Fonfría, Víctor; Gutierrez-Gallego, Ricardo; Jerónimo, Celia; Iturbide, Ane; Di Croce, Luciano; García de Herreros, Antonio; Peiró, Sandra

    2016-12-01

    Methylation of histone H3 lysine 4 is linked to active transcription and can be removed by LSD1 or the JmjC domain-containing proteins by amino-oxidation or hydroxylation, respectively. Here we describe that its deamination can be catalyzed by lysyl oxidase-like 2 protein (LOXL2), presenting an unconventional chemical mechanism for H3K4 modification. Infrared spectroscopy and mass spectrometry analyses demonstrated that recombinant LOXL2 specifically deaminates trimethylated H3K4. Moreover, by regulating H3K4me3 deamination, LOXL2 activity is linked with the transcriptional control of the CDH1 gene. These results reveal the existence of further H3 modification as well as a novel mechanism for H3K4me3 demethylation.

  16. 5,6-Dihydro-2H-1,3-dithiolo[4,5-b][1,4]dioxine-2-thione

    PubMed Central

    Wang, Guan-nan; Xiao, Xun-wen; Cai, Tongjiang; Huang, Qin

    2011-01-01

    The title mol­ecule, C5H4O2S3, consists of a planar [mean deviation = 0.020 (1) Å] 1,3-dithiole-2-thione unit with an ethyl­enedi­oxy group in the 4,5-positions. The dioxine ring is in a twist-chair conformation. PMID:21754789

  17. 5,6-Dihydro-2H-1,3-dithiolo[4,5-b][1,4]dioxine-2-thione.

    PubMed

    Wang, Guan-Nan; Xiao, Xun-Wen; Cai, Tongjiang; Huang, Qin

    2011-06-01

    The title mol-ecule, C(5)H(4)O(2)S(3), consists of a planar [mean deviation = 0.020 (1) Å] 1,3-dithiole-2-thione unit with an ethyl-enedi-oxy group in the 4,5-positions. The dioxine ring is in a twist-chair conformation.

  18. Development of 6H-Chromeno[3,4-c]pyrido[3',2':4,5]thieno[2,3-e]pyridazin-6-ones as Par-4 Secretagogues

    PubMed Central

    Frasinyuk, Mykhaylo S.; Bondarenko, Svitlana P.; Sviripa, Vitaliy M.; Burikhanov, Ravshan; Rangnekar, Vivek M.; Liu, Chunming; Watt, David S.

    2015-01-01

    Nitrosation and cyclization of 4-(3-aminothieno[2,3-b]pyridine-2-yl)-2H-chromen-2-ones 1 afforded substituted 6H-chromeno[3,4-c]pyrido[3',2':4,5]thieno[2,3-e]pyridazin-6-ones 2 that inhibited the intermediary filament protein, vimentin, at low micromolar concentrations. This inhibition promoted the secretion of Prostate Apoptosis Response-4 protein (Par-4), which selectively triggered apoptosis in prostate cancer cells such as CWR22Rv1, LNCaP-derivative C4-2B, PC-3 and its aggressive analog, PC-3 MM2. PMID:26236052

  19. Synthesis, antimicrobial activity and QSAR studies of new 2,3-disubstituted-3,3a,4,5,6,7-hexahydro-2H-indazoles.

    PubMed

    Minu, Maninder; Thangadurai, Ananda; Wakode, Sharad Ramesh; Agrawal, Shyam Sundar; Narasimhan, Balasubramanian

    2009-06-01

    Antimicrobial activity of synthesized 2,3-disubstituted-3,3a,4,5,6,7-hexahydro-2H-indazole derivatives indicated that 3-(4-chlorophenyl)-2-(4-nitrophenylsulfonyl)-3,3a,4,5,6,7-hexahydro-2H-indazole (6) and 3-(4-fluorophenyl)-2-(4-nitrophenylsulfonyl)-3,3a,4,5,6,7-hexahydro-2H-indazole (20) were the most active compounds. Further, the results of QSAR studies indicated the importance of topological parameters (2)chi and (2)chi(v) in defining the antimicrobial activity of hexahydroindazoles.

  20. Synthesis of Novel 2,5-Disubstituted-1,3,4-thiadiazoles Clubbed 1,2,4-Triazole, 1,3,4-Thiadiazole, 1,3,4-Oxadiazole and/or Schiff Base as Potential Antimicrobial and Antiproliferative Agents.

    PubMed

    Rezki, Nadjet; Al-Yahyawi, Amjad M; Bardaweel, Sanaa K; Al-Blewi, Fawzia F; Aouad, Mohamed R

    2015-09-02

    In the present study, a new series of 2,5-disubstituted-1,3,4-thiadiazole tethered 1,2,4-triazole, 1,3,4-thiadiazole, 1,3,4-oxadiazole and Schiff base derivatives were synthesized and characterized by IR, ¹H-NMR, (13)C-NMR, MS and elemental analyses. All compounds were screened for their antibacterial, antifungal and antiproliferative activity. Some of the synthesized derivatives have displayed promising biological activity.

  1. Variation of properties of glasses along the 3Bi2O3 X 5B2O3-4PbO X B2O3 and PbO X 2B2O3-2PbO X Bi2O3 sections of the PbO-Bi2O3-B2O3 ternary system

    SciTech Connect

    Zargarova, M.I.; Shuster, N.S.

    1985-07-01

    Already published data on the phase diagrams of Pb-B2O3, Bi2O3-B2O3, and PbO-Bi2O3 systems serve as the basis of this investigation, together with original experiments on the PbO-Bi2O3-B2O3 ternary system. The authors establish the quasi binary nature of the 3Bi2O3 X 5B2O3 - 4PbO X B2O3 section with the formation of the congruently melting ternary compound 3Bi2O3 X 8PbO X 7B2O3, and they demonstrate the role of the ternary compound 3Bi2O3 X 8PbO X 7B2O3 as a glass former in the PbO-Bi2O3 - B2O3 system.

  2. [1,2,4]triazolo[4,3-a]phthalazines: inhibitors of diverse bromodomains.

    PubMed

    Fedorov, Oleg; Lingard, Hannah; Wells, Chris; Monteiro, Octovia P; Picaud, Sarah; Keates, Tracy; Yapp, Clarence; Philpott, Martin; Martin, Sarah J; Felletar, Ildiko; Marsden, Brian D; Filippakopoulos, Panagis; Müller, Susanne; Knapp, Stefan; Brennan, Paul E

    2014-01-23

    Bromodomains are gaining increasing interest as drug targets. Commercially sourced and de novo synthesized substituted [1,2,4]triazolo[4,3-a]phthalazines are potent inhibitors of both the BET bromodomains such as BRD4 as well as bromodomains outside the BET family such as BRD9, CECR2, and CREBBP. This new series of compounds is the first example of submicromolar inhibitors of bromodomains outside the BET subfamily. Representative compounds are active in cells exhibiting potent cellular inhibition activity in a FRAP model of CREBBP and chromatin association. The compounds described are valuable starting points for discovery of selective bromodomain inhibitors and inhibitors with mixed bromodomain pharmacology.

  3. [1,2,4]Triazolo[4,3-a]phthalazines: Inhibitors of Diverse Bromodomains

    PubMed Central

    2013-01-01

    Bromodomains are gaining increasing interest as drug targets. Commercially sourced and de novo synthesized substituted [1,2,4]triazolo[4,3-a]phthalazines are potent inhibitors of both the BET bromodomains such as BRD4 as well as bromodomains outside the BET family such as BRD9, CECR2, and CREBBP. This new series of compounds is the first example of submicromolar inhibitors of bromodomains outside the BET subfamily. Representative compounds are active in cells exhibiting potent cellular inhibition activity in a FRAP model of CREBBP and chromatin association. The compounds described are valuable starting points for discovery of selective bromodomain inhibitors and inhibitors with mixed bromodomain pharmacology. PMID:24313754

  4. K(MoO2)4O3(AsO4)

    PubMed Central

    Jouini, Raja; Zid, Mohamed Faouzi; Driss, Ahmed

    2013-01-01

    A new compound with a non-centrosymmetric structure, potassium tetra­kis­[dioxomolybdenum(IV)] arsenate trioxide, K(MoO2)4O3(AsO4), has been synthesized by a solid-state reaction. The [(MoO2)4O3(AsO4)]+ three-dimensional framework consists of single arsenate AsO4 tetra­hedra, MoO6 octa­hedra, MoO5 bipyramids and bi­octa­hedral units of edge-sharing Mo2O10 octa­hedra. The [Mo2O8]∞ octa­hedral chains running along the a-axis direction are connected through their corners to the AsO4 tetra­hedra, MoO6 octa­hedra and MoO5 bipyramids, so as to form large tunnels propagating along the a axis in which the K+ cations are located. This structure is compared with compounds containing M 2O10 (M = Mo, V, Fe) dimers and with those containing M 2O8 (M = V) chains. PMID:23794968

  5. Lattice dynamics of La 2CuO 4 and YBa 2Cu 3O 7

    NASA Astrophysics Data System (ADS)

    Kimura, Shunji; Sota, Takayuki; Suzuki, Katsuo

    1990-08-01

    We report lattice dynamics calculations of La 2CuO 4 and YBa 2Cu 3O 7 where the mode assignment is fully performed. It is found that frequencies of the in-plane bond streching 0 vibration mode phonons are much higher than those of the bond bending 0 vibration mode phonons in La 2CuO 4 while they are close in YBa 2Cu 3O 7. The bond streching mode phonons and the bond bending mode phonons can couple to electrons near E F in YBa 2Cu 3O 7 but the latter can not in La 2CuO 4.

  6. Modulated magnetism and anomalous electronic transport in Ce3Cu4As4O2

    NASA Astrophysics Data System (ADS)

    Wang, Jiakui K.; Wu, Shan; Qiu, Yiming; Rodriguez-Rivera, Jose A.; Huang, Qingzhen; Broholm, C.; Morosan, E.

    2016-08-01

    The complex magnetism and transport properties of tetragonal Ce3Cu4As4O2 were examined through neutron scattering and physical property measurements on polycrystalline samples. The lamellar structure consists of alternating layers of CeCu4As4 with a single square Ce lattice and Ce2O2 bilayers. Peaks in the specific heat at the Néel temperature TN=24 K, T2=16 K, and T3=1.9 K indicate three magnetic phase transitions or distinct crossover phenomena. For T 2 , quasi-two-dimensional low-energy spin fluctuations with k2=1/2 a* and polarized perpendicular to k2 are suppressed. The data are consistent with quasi-two-dimensional antiferromagnetic order in the CeCu4As4 planes polarized along the k2 wave vector. T3 marks a spin-flop transition where the k1 staggered magnetization switches to in-plane polarization. There are significant transport anomalies associated with the transitions, in particular a substantial reduction in resistivity for T 2 K. We trace the unusual sequence of magnetic transitions to competing interactions and anisotropies in the alternating quasi-two-dimensional magnetic layers.

  7. Synthesis, characterization and stereochemistry of N-acyl-r-2,c-4-bis(4-methoxyphenyl)-3-azabicyclo[3.3.1]nonanes

    NASA Astrophysics Data System (ADS)

    Akila, A.; Ponnuswamy, S.; Shreevidhyaa Suressh, V.; Usha, G.

    2015-08-01

    Four new N-acyl-2,4-bis(4-methoxyphenyl)-3-azabicyclo[3.3.1]nonanes 3-6 have been synthesized. The structural characterization and the conformational preferences of the compounds 3-6 have been carried out using IR, 1D and 2D NMR and Mass spectral data. The NMR spectral data indicates that the N-acyl-2,4-bis(4-methoxyphenyl)-3-azabicyclo[3.3.1]nonanes 3-6 prefer to exist in twin-chair conformation with partial flattening at nitrogen end. To avoid A1,3-strain, the anisyl groups at C2 and C4 are forced to occupy the quasi-axial orientation. X-ray crystal structure of the N-dichloroacetyl-2,4-bis(4-methoxyphenyl)-3-azabicyclo[3.3.1]nonane 6 also supports the similar conformation in the solid state.

  8. Antiinflammatory 2-benzyl-4-sulfonyl-4H-isoquinoline-1,3-diones: novel inhibitors of COX-2.

    PubMed

    Lazer, E S; Sorcek, R; Cywin, C L; Thome, D; Possanza, G J; Graham, A G; Churchill, L

    1998-05-19

    A series of 2-benzyl-4-sulfonyl-4H-isoquinoline-1,3-diones was prepared. Members of this series are potent and selective inhibitors of cyclooxygenase-2 (COX-2) in both microsomal and cellular assays. Two representatives demonstrated activity in the carrageenan-induced paw edema model in rats upon oral administration.

  9. Fluorination of 1,2,3,4- and 1,2,3,5-tetrahalobenzenes with potassium fluoride in dimethyl sulfone

    USGS Publications Warehouse

    Finger, G.C.; Dickerson, D.R.; Shiley, R.H.

    1972-01-01

    1,2,3,4-Tetrachlorobenzene, 1,2,3,5-tetrachlorobenzene, 2,4,6-trichlorofluorobenzene, and 2,6-dichloro-1,4-difluorobenzene were fluorinated with potassium fluoride and potassium fluoride-cesium fluoride mixtures in dimethyl sulfone. By varying the concentration, temperature and reaction time, the degree of fluorination could be controlled to some extent. The optimum conditions for producing mono-, di- and tri-fluoro-substituted chlorobenzenes and trace amounts of tetrafluorobenzene from the corresponding tetrachlorobenzenes are given. 1,2,3,5-Tetrafluorobenzene was obtained in 44.8% yield from 2,6-dichloro-1,4-difluorobenzene. 1,2,3,4-Tetrafluorobenzene was obtained in only trace amounts from 1,2,3,4-tetrachlorobenzene. A total of 24 new chlorofluorobenzenes and intermediates are described. Fluorination with potassium fluoride and certain other metal fluorides was also investigated. ?? 1972.

  10. 1-Methyl-4H-3,1-benzoxazine-2,4(1H)dione

    PubMed Central

    Deifel, Nicholas P.; Cherney, Emily; Hunt, David A.; Chan, Benny C.

    2010-01-01

    In its crystal structure, the title compound, C9H7NO3, forms π-stacked dimers, with a centroid–centroid distance of 3.475 (5) Å between the benzenoid and the 2,4 dicarbonyl oxazine rings. These dimers then form staircase-like linear chains through further π-stacking between the benzenoid rings [centroid–centroid distance of 3.761 (2) Å]. The methyl-H atoms are disordered due to rotation about the C—N bond and were modeled with equal occupancy. PMID:21580413

  11. Pressure sintering of Si3N4-Al2O3 /Sialon/

    NASA Technical Reports Server (NTRS)

    Yeh, H. C.; Sanders, W. A.; Fiyalko Luttner, J. L.

    1977-01-01

    Essentially pore-free Sialon bodies were obtained by pressure sintering for three blends (mol ratios of 4:1, 2:3, and 3:2) of Si3N4 and Al2O3 powders under the conditions of 27.6 MN/sq m and a temperature of 1700 C for 2 h. These dense bodies consist mainly of a Sialon solid solution with a minor amount of a particular second phase. The higher the Al2O3 content (20 to 60 mol% range) in Sialon, the higher the densification rate. Fully dense bodies can be obtained at temperatures as low as 1500 C at 27.6 MN/sq m for 2 h with no second phase detectable by X-ray diffraction. A 100% dense body can be obtained by heating at 1700 C at 27.6 MN/sq m without a holding time.

  12. Moessbauer studies in Zn(2+)0.3 Mn(2+)0.7 Mn(3+) (2-y) Fe(3+) (2-y) O4

    NASA Technical Reports Server (NTRS)

    Gupta, R. G.; Mendiratta, R. G.; Escue, W. T.

    1975-01-01

    The Mossbauer effect has proven to be effective in the study of nuclear hyperfine interactions. Ferrite systems having the formula (Zn(2+)0.3)(Mn(2+)0.7)(Mn(3+)y)(Fe(3+)2-y)(O4) were prepared and studied. These systems can be interpreted as mangacese-doped zinc and a part of iron ions. A systematic study of these systems is presented to promote an understanding of their microstructure for which various theories were proposed.

  13. Synthesis and biological activities of novel furo[2,3,4-jk][2]benzazepin-4(3H)-one derivatives.

    PubMed

    Ando, Kumiko; Akai, Yukiko; Kunitomo, Jun-Ichi; Yokomizo, Takehiko; Nakajima, Hidemitsu; Takeuchi, Tadayoshi; Yamashita, Masayuki; Ohta, Shunsaku; Ohishi, Takahiro; Ohishi, Yoshitaka

    2007-02-21

    A novel seven-membered lactam formation method has been established by intramolecular ring closure reaction of 4-bromo-(E)-3-[(2-alkylvinyl)carbonylamino]benzo[b]furans under Heck coupling conditions. A number of furo[2,3,4-jk][2]benzazepin-4(3H)-ones, tricyclicbenzo[b]furans, have been prepared by this method and evaluated for their leukotriene B(4) (LTB(4)) receptor and poly(ADP-ribose)polymerase-1 (PARP-1) inhibitory activities.

  14. Molecular structures of antiviral agents, 2,3-dihydroxybenzaldehyde 2,4-dinitrophenylhydrazone and 4-[(4-methylpiperazin-1-yl)imino]methyl-1,2-benzodiol

    SciTech Connect

    Gurskaya, G. V.; Zavodnik, V. E.; Zhukhlistova, N. E.; Kozlov, M. V.

    2008-07-15

    Two antiviral agents, namely, 2,3-dihydroxybenzaldehyde 2,4-dinitrophenylhydrazone and 4-[(4-methylpiperazin-1-yl)imino]methyl-1,2-benzodiol, are studied by X-ray diffraction. The stereochemical features of the molecular structures of the compounds under investigation are discussed, and the possible correlation between the structure and biological activity with respect to hepatitis C virus RNA-dependent RNA polymerase is analyzed.

  15. Immiscibility in the Fe3O4-FeCr2O4 Spinel Binary

    SciTech Connect

    S.E. Ziemniak; R.A. Castelli

    2003-03-20

    A recent thermodynamic model of mixing in spinel binaries, based on changes in cation disordering (x) between tetrahedral and octahedral sites, is investigated for applicability to the Fe{sub 3}O{sub 4}-FeCr{sub 2}O{sub 4} system under conditions where incomplete mixing occurs. Poor agreement with measured consolute solution temperature and solvus is attributed to neglect of: (1) ordering of magnetic moments of cations in the tetrahedral sublattice antiparallel to the moments of those in the octahedral sublattice and (2) pair-wise electron hopping between octahedral site Fe{sup 3+} and Fe{sup 2+} ions. Disordering free energies ({Delta}G{sub D}), from which free energies of mixing are calculated, are modeled by {Delta}G{sub D} = {alpha}{chi} + {beta}{chi}{sup 2} - T(S{sub c} + {chi}{sigma}{sub el} + {gamma}{chi}{sigma}{sup mag}) where the previously-neglected effects are accommodated by: (1) adding a non-configurational entropy term to provide coupling between cation disordering and magnetic ordering and (2) revising the configurational entropy (S{sub c}) analysis. Applying the constraint {alpha} = -(2/3){beta} and regressing the existing database for Fe{sup 2+} ion disorder in Fe{sub 3}O{sub 4} gives: {beta} = -31,020 {+-} 1050 J mol{sup -1}, {sigma}{sub el}/R = -0.730 {+-} 0.081 and {gamma}, the coupling parameter between cation disordering and magnetic ordering, = -0.664 {+-} 0.075. The revised mixing model predicts a consolute solution temperature (T{sub cs}) = 600 C and a solvus at 500 C of n = 0.05 and 0.70 for the Fe(Fe{sub 1-n}Cr{sub n}){sub 2}O{sub 4} spinel binary.

  16. 5,7-Di-2-pyridyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine.

    PubMed

    Djukic, Brandon; Harrington, Laura E; Britten, James F; Lemaire, Martin T

    2008-01-16

    The title compound, C(16)H(12)N(2)O(2)S, was prepared by a Neigishi cross-coupling reaction to investigate the coordination chemistry of thio-phene-containing ligands. In the mol-ecule, the pyridine rings are twisted from the thio-phene ring by 20.6 (1) and 4.1 (2)°. The six-membered dihydro-dioxine ring is in a half-chair conformation.

  17. 1-[2-(4-Chloro­phen­yl)-5-phenyl-2,3-dihydro-1,3,4-oxadiazol-3-yl]ethanone

    PubMed Central

    Fun, Hoong-Kun; Arshad, Suhana; Shyma, P. C.; Kalluraya, Balakrishna; Arulmoli, T.

    2012-01-01

    In the title compound, C16H14ClN3O2, the 2,3-dihydro-1,3,4-oxadiazole ring [maximum deviation = 0.030 (1) Å] and the pyridine ring [maximum deviation = 0.012 (1) Å] are inclined slightly to one another, making a dihedral angle of 11.91 (5)°. The chloro-substituted phenyl ring is almost perpendicular to the 2,3-dihydro-1,3,4-oxadiazole and pyridine rings at dihedral angles of 86.86 (5) and 75.26 (5)°, respectively. In the crystal, π–π [centroid–centroid distance = 3.7311 (6) Å] and C—H⋯π inter­actions are observed. PMID:22719656

  18. Transcription in the absence of histone H3.2 and H3K4 methylation.

    PubMed

    Hödl, Martina; Basler, Konrad

    2012-12-04

    Histone H3 proteins play fundamental roles in DNA packaging, gene transcription, and the transmission of epigenetic states. In addition to posttranslational modifications of their N termini, the use of H3 variants contributes to their regulatory repertoire. Canonical histone H3.2 is expressed during S phase and differs by four amino acid residues from the variant histone H3.3, which is synthesized in a cell-cycle-independent manner. Because H3.3 is enriched within actively transcribed loci, and because di- and trimethylation of H3 lysine 4 are hallmarks of chromatin at such sites in the genome, the H3.3K4 residue is considered to serve as the major regulatory determinant for the transcriptional state of a gene. Here we use genetic approaches in Drosophila to replace all 46 gene copies of His3.2 with mutant derivatives and thereby demonstrate that canonical and variant H3 can functionally replace each other. Cells are able to divide and differentiate when H3.2 is entirely absent but replaced by S phase-expressed H3.3. Moreover, although slowed down in their proliferative capacity, cells that code for a nonmethylatable residue instead of K4 in all canonical and variant H3 genes are competent to respond to major developmental signaling pathways by activating target gene expression. Hence, the presence of different H3 protein species is not essential in Drosophila and transcriptional regulation can occur in the complete absence of H3K4 methylation.

  19. The Unique α4(+)/(−)α4 Agonist Binding Site in (α4)32)2 Subtype Nicotinic Acetylcholine Receptors Permits Differential Agonist Desensitization Pharmacology versus the (α4)22)3 Subtype

    PubMed Central

    Eaton, J. Brek; Lucero, Linda M.; Stratton, Harrison; Chang, Yongchang; Cooper, John F.; Lindstrom, Jon M.; Lukas, Ronald J.

    2014-01-01

    Selected nicotinic agonists were used to activate and desensitize high-sensitivity (HS) (α4)22)3) or low-sensitivity (LS) (α4)32)2) isoforms of human α4β2-nicotinic acetylcholine receptors (nAChRs). Function was assessed using 86Rb+ efflux in a stably transfected SH-EP1-hα4β2 human epithelial cell line, and two-electrode voltage-clamp electrophysiology in Xenopus laevis oocytes expressing concatenated pentameric HS or LS α4β2-nAChR constructs (HSP and LSP). Unlike previously studied agonists, desensitization by the highly selective agonists A-85380 [3-(2(S)-azetidinylmethoxy)pyridine] and sazetidine-A (Saz-A) preferentially reduced α4β2-nAChR HS-phase versus LS-phase responses. The concatenated-nAChR experiments confirmed that approximately 20% of LS-isoform acetylcholine-induced function occurs in an HS-like phase, which is abolished by Saz-A preincubation. Six mutant LSPs were generated, each targeting a conserved agonist binding residue within the LS-isoform-only α4(+)/(−)α4 interface agonist binding site. Every mutation reduced the percentage of LS-phase function, demonstrating that this site underpins LS-phase function. Oocyte-surface expression of the HSP and each of the LSP constructs was statistically indistinguishable, as measured using β2-subunit–specific [125I]mAb295 labeling. However, maximum function is approximately five times greater on a “per-receptor” basis for unmodified LSP versus HSP α4β2-nAChRs. Thus, recruitment of the α4(+)/(−)α4 site at higher agonist concentrations appears to augment otherwise-similar function mediated by the pair of α4(+)/(−)β2 sites shared by both isoforms. These studies elucidate the receptor-level differences underlying the differential pharmacology of the two α4β2-nAChR isoforms, and demonstrate that HS versus LS α4β2-nAChR activity can be selectively manipulated using pharmacological approaches. Since α4β2 nAChRs are the predominant neuronal subtype, these discoveries likely

  20. Reaction of 2,2,4,4-tetrakis(trifluoromethyl)-1,3-dithiethane with N-vinyl compounds.

    PubMed

    Petrov, Viacheslav A; Marshall, Will

    2013-01-01

    The reaction of hexafluorothioacetone dimer (2,2,4,4-tetrakis(trifluoromethyl)-1,3-dithiethane, 1) with vinylamides leads to the rapid formation of [2 + 2] cycloadducts: 4-amino-2,2-bis(trifluoromethyl)thietanes. The reaction proceeds in polar solvents (DMF, DMSO) in the absence of a catalyst at elevated temperature producing the corresponding cycloadducts in 47-86% yield. The reaction of N-vinylimidazole unexpectedly led to the formation of the corresponding 1-(hexafluoroisopropyl)-3-vinyl-1,3-dihydro-2H-imidazole-2-thione (5). The structure of this compound, along with the structures of two new thietanes was confirmed by single crystal X-ray diffraction.

  1. Enantiomeric separation of racemic 4-aryl-1,4-dihydropyridines and 4-aryl-1,2,3,4-tetrahydropyrimidines on a chiral tetraproline stationary phase.

    PubMed

    Dai, Zhi; Pittman, Charles U; Li, Tingyu

    2013-04-01

    The chromatographic chiral resolution of 4-aryl-1,4-dihydropyridines (1-32), 4-aryl-2-thioxo-1,2,3,4-tetrahydropyrimidines (33-38), and 4-aryl-2-oxo-1,2,3,4-tetrahydropyrimidines (39-41) was studied on a tetraproline-immobilized chiral column synthesized in our lab. This tetraproline chiral stationary phase can resolve most of these compounds. The 4-aryl-2-thioxo-1,2,3,4-tetrahydropyrimidines (33-38) and 4-aryl-2-oxo-1,2,3,4-tetrahydropyrimidines (39-41) were more efficiently resolved than the racemic 4-aryl-1,4-dihydropyridines on the tetraproline chiralstationary phase. Analytes with 5,5-dimethyl groups (39-41) were less efficiently resolved than analytes without 5,5-dimethyl substituents (1-16). The 4-aryl-2-oxo-1,2,3,4-tetrahydropyrimidines (39-41) without a sulfur atom were much more efficiently resolved than 4-aryl-2-thioxo-1,2,3,4-tetrahydropyrimidines (33-38). No obvious electronic effects on the resolution of any of these analytes (1-41) were observed on the tetraproline chiral stationary phase. The tetraproline chiral stationary phase separated enantiomers mainly via hydrogen bonding interactions.

  2. The Hydrothermal NH 4/V/P/H 2O and K/v/p/n(c 2H 5) 3/H 2O Systems at 473 K and the Crystal Structures of NH 4VOPO 4and (nh 4) 3V 2O 3(VO)(PO 4) 2(HPO 4)

    NASA Astrophysics Data System (ADS)

    Schindler, Michael; Joswig, Werner; Baur, Werner H.

    1997-12-01

    An examination of the NH 4/VO 5/P/H 2O system at 473 K under hydrothermal conditions yielded the (NH 4) 3V 2O 3(VO)(PO 4) 2(HPO 4) and NH 4VOPO 4phases. The crystal structure of the first compound is isotypical with the corresponding Tl +and K +phases. The cations NH +4and Tl +have similar coordinations against oxygen. The investigation of the crystal structure of the second compound (space group Pn2 n) shows it to be related to other ABO TO 4phases of the potassium titanyl phosphate type with A=Na +, Ag +, NH +4, Rb +, K +, and Tl +, and B=Ti 4+, V 4+, Sn 4+, Fe 4+, Ge 4+, Ga 3+, Zr 4+, Sb 5+, and Nb 5+, and T=P 5+, Ge 4+, Si 4+, and As 5+, but none of them crystallize in space group Pn2 n. In the K/V/P/N(C 2H 5) 3/H 2O system, three different K phases were found: K 0.5VOPO 4·1.5H 2O, KVOPO 4, and K-FVP-1 (Frankfurt vanadium phosphate, one, or for short, FVP-1). The microporous K-FVP-1 compound was synthesized in a similar pH range as the isotypic Na-FVP-1 phase. The V 4+/V 5+ratio of K-FVP-1 varies from 3.5(1)/1.5(1) to 1.6(1)/3.4(1) and the corresponding lattice constants range from 16.0013(6) to 15.7665(4) Å.

  3. Cyclic sulfoxides garlicnins B2, B3, B4, C2, and C3 from Allium sativum.

    PubMed

    Nohara, Toshihiro; Fujiwara, Yukio; Ikeda, Tsuyoshi; Murakami, Kohtaro; Ono, Masateru; Nakano, Daisuke; Kinjo, Junei

    2013-01-01

    Several novel sulfides, called garlicnins B2 (1), B3 (2), B4 (3), C2 (4), and C3 (5), were isolated from acetone extracts of garlic, Allium sativum L. and characterized. These garlicnins are capable of suppressing M2 macrophage activation and they have a novel skeleton of cyclic sulfoxide. The structures of the former 3 and latter of 2 were deduced to be 2-(sulfenic acid)-5-(allyl)-3,4-dimethyltetrahydrothiophene-S-oxides and 2-(allyldithiine)-5-(propenylsulfoxide)-3,4-dimethyltetrahydrothiophene-S-oxides, respectively. The mechanism of the proposed production of these compounds is discussed. The identification of these novel sulfoxides from garlic accumulates a great deal of new chemistry in the Allium sulfide field, and future pharmacological investigations of these compounds will aid the development of natural, healthy foods and anti-cancer agents that may prevent or combat disease.

  4. Synthesis and crystal chemistry of two new fluorite-related bismuth phosphates, Bi(4.25)(PO4)2O(3.375) and Bi5(PO4)2O4.5, in the Series Bi4+x(PO4)2O3+3x/2 (0.175 < or = x < or = 1).

    PubMed

    Muktha, B; Guru Row, T N

    2006-06-12

    Two new phosphates, Bi(4.25)(PO4)2O(3.375) and Bi(5)(PO(4))(2)O(4.5), have been analyzed by single-crystal X-ray diffraction in the series Bi(4+x)(PO4)2O(3+3x/2) (0.175 < or = x < or = 1). The syntheses of the compositions ranging from x = 0.175 to 0.475 were carried out by the ceramic route. The compositions from x = 0.175 to 0.475 form a solid solution with a structure similar to that of Bi(4.25)(PO4)2O(3.375), while Bi(5)(PO4)2O(4.5) was isolated from a mixture of two phases. Both of the phases form fluorite-related structures but, nevertheless, differ from each other with respect to the arrangement of the bismuth atoms. The uniqueness in the structures is the appearance of isolated PO(4) tetrahedra separated by interleaving [Bi2O2] units. ac impedance studies indicate conductivity on the order of 10(-5) S cm(-1) for Bi(4.25)(PO4)2O(3.375). Crystal data: Bi(4.25)(PO4)2O(3.375), triclinic, space group P (No. 1), with a = 7.047(1) A, b = 9.863(2) A, c = 15.365(4) A, alpha = 77.604(4) degrees, beta = 84.556(4) degrees, gamma = 70.152(4) degrees, V = 980.90(4) A3, and Z = 4; Bi(5)(PO4)2O(4.5), monoclinic, space group C2/c (No. 15), with a = 13.093(1) A, b = 5.707(1) A, c = 15.293(1) A, beta = 98.240(2) degrees, V = 1130.95(4) A(3), and Z = 8.

  5. Synthesis and crystal structure of 2-(4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol

    NASA Astrophysics Data System (ADS)

    Li, S.-J.; Shen, D.; Zhang, C.-Z.

    2015-11-01

    The title compound 2-(4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol was synthesized by the reaction of phenol with hexafluoroacetone using mesitylene as solvent and. methanesulfonic acid as catalist. The structure is determined by X-ray structure analysis. Two kinds of strong intermolecular hydrogen bonds O( Alk)-H···O( Ar)and O( Ar)-H···O( Alk) are formed in crystal. These hydrogen bonds connect the molecules into two-dimensional layers. Based on theoretical calculations of the electronic structure of the title compound, its application in fluoro-containing materials is predicted. The title compound may be employed to synthesize many organic fluoro-containing polymers, because alcoholic hydroxyl and phenolic hydroxyl are easily deprotonated.

  6. Preparation of 1,1'-dinitro-3,3'-azo-1,2,4-triazole

    DOEpatents

    Lee, Kien-Yin

    1986-01-01

    A new high density composition of matter, 1,1'-dinitro-3,3'-azo-1,2,4-triazole, has been synthesized using inexpensive, commonly available compounds. This compound has been found to be an explosive, and its use as a propellant is anticipated.

  7. Polyimides from 2,3,3',4'-Biphenyltetracarboxylic Dianhydride and Aromatic Diamines

    NASA Technical Reports Server (NTRS)

    Hergenrother, Paul M. (Inventor); Smith, Joseph G. (Inventor); Connell, John W. (Inventor); Watson, Kent A. (Inventor)

    2005-01-01

    The present invention relates generally to polyimides. It relates particularly to novel polyimides prepared from 2,3, 3',4' -biphenyltetracarboxylic dianhydride and aromatic diamines. These novel polyimides have low color, good solubility, high thermal emissivity, low solar absorptivity and high tensile strength.

  8. Preparation of 3,3'-azobis(6-amino-1,2,4,5-tetrazine)

    DOEpatents

    Hiskey, Michael A.; Chavez, David E.; Naud, Darren

    2002-01-01

    The compound of the structure ##STR1## where a, b, c, d and e are 0 or 1 and a+b+c+d+e is from 0 to 5 is disclosed together with the species 3,3'-azobis(6-amino-1,2,4,5-tetrazine) and a process of preparing such compounds.

  9. Broadband Yellowish-Green Emitting Ba4Gd3Na3(PO4)6F2:Eu(2+) Phosphor: Structure Refinement, Energy Transfer, and Thermal Stability.

    PubMed

    Fu, Xiaopeng; Lü, Wei; Jiao, Mengmeng; You, Hongpeng

    2016-06-20

    A series of Ba4Gd3Na3(PO4)6F2:Eu(2+) phosphors with a broad emitting band have been synthesized by a traditional solid state reaction. The crystal structural and photoluminescence properties of Ba4Gd3Na3(PO4)6F2:Eu(2+) are investigated. The different crystallographic sites of Eu(2+) in Ba4Gd3Na3(PO4)6F2:Eu(2+) phosphors have been verified by means of their photoluminescence (PL) properties and decay times. Energy transfer between Eu(2+) ions, analyzed by excitation, emission, and PL decay behavior, has been indicated to be a dipole-dipole mechanism. Moreover, the luminescence quantum yield as well as the thermal stability of the Ba4Gd3Na3(PO4)6F2:Eu(2+) phosphor have been investigated systematically. The as-prepared Ba4Gd3Na3(PO4)6F2:Eu(2+) phosphor can act as a promising candidate for n-UV convertible white LEDs.

  10. 2,6-Dihy-droxy-4-oxo-2-(pyridin-1-ium-3-yl)-4H-1,3,2-benzodioxaborinin-2-ide 0.67-hydrate.

    PubMed

    Garcia-Grajeda, Blanca A; Höpfl, Herbert; Guerrero-Alvarez, Jorge A; Campos-Gaxiola, José J; Cruz-Enríquez, Adriana

    2014-04-01

    The asymmetric unit of the title compound, C12H10BNO5·0.67H2O, contains three independent pyridinylboronic acid esters adopting zwitterionic forms and two water mol-ecules. The six-membered heterocyclic rings in the boronic esters have half-chair conformations and the deviations of the B atoms from the boronate mean planes range from 0.456 (3) to 0.657 (3) Å. All of the B atoms have tetra-hedral coordination environments, with B-O and B-C bond lengths of 1.446 (4)-1.539 (3) and 1.590 (5)-1.609 (5) Å, respectively. In the crystal, the ester and water mol-ecules are linked into a three-dimensional network by a large number of O-H⋯O, N-H⋯O and C-H⋯O hydrogen bonds. The crystal packing is further accomplished by π-π inter-actions, with centroid-centroid distances of 3.621 (4)-3.787 (4) Å.

  11. Transition probabilities for the 3s2 3p(2P0)-3s3p2(4P) intersystem lines of Si II

    NASA Technical Reports Server (NTRS)

    Calamai, Anthony G.; Smith, Peter L.; Bergeson, S. D.

    1993-01-01

    Intensity ratios of lines of the spin-changing 'intersystem' multiplet of S II (4P yields 2P0) at 234 nm have been used to determine electron densities and temperatures in a variety of astrophysical environments. However, the accuracy of these diagnostic calculations have been limited by uncertainties associated with the available atomic data. We report the first laboratory measurement, using an ion-trapping technique, of the radiative lifetimes of the three metastable levels of the 3s3p2 4P term of Si II. Our results are 104 +/- 16, 406 +/- 33, and 811 +/- 77 micro-s for lifetimes of the J = 1/2, 5/2, and 3/2 levels, respectively. A-values were derived from our lifetimes by use of measured branching fractions. Our A-values, which differ from calculated values by 30 percent or more, should give better agreement between modeled and observed Si II line ratios.

  12. Autioionizing states in the photionization of the 3s(2)3p(4) (3)Pe ground state of sulfur

    NASA Technical Reports Server (NTRS)

    Tayal, S. S.

    1988-01-01

    The partial and total photoionization cross sections for the S(3s/2/3p/4/ /3/Pe) ground state are calculated in both the dipole length and velocity forms. The prominent features in the cross sections are the autoionization Rydberg series converging to S+(3s/2/p/3/ /2/D/0/, /2/P/0/) excited-state thresholds. The results are pertinent to the study of sulfur in the plasma of Jupiter's satellite Io.

  13. 11H-Pyrido[3',2':4,5]pyrrolo[3,2-c]cinnoline and pyrido[3',2':4,5]pyrrolo[1,2-c][1,2,3]benzotriazine: two new ring systems with antitumor activity.

    PubMed

    Parrino, Barbara; Carbone, Anna; Muscarella, Marina; Spanò, Virginia; Montalbano, Alessandra; Barraja, Paola; Salvador, Alessia; Vedaldi, Daniela; Cirrincione, Girolamo; Diana, Patrizia

    2014-11-26

    Derivatives of new ring systems 11H-pyrido[3',2':4,5]pyrrolo[3,2-c]cinnoline and pyrido[3',2':4,5]pyrrolo[1,2-c][1,2,3]benzotriazine have been prepared from the key intermediates 2-(1H-pyrrolo[2,3-b]pyridin-2-yl)anilines in excellent yields (94-99%) and screened by the National Cancer Institute (Bethesda, MD) on about 60 human tumor cell lines derived from nine cancer cell types. The tested compounds exhibited antiproliferative activity against all the human cell lines, showing comparable MG_MID (mean graph midpoint) values in the range of 0.74-1.15 μM. A particular efficacy was observed against the leukemia subpanel (GI50 = 0.73-0.0090 μM). Flow cytometric analysis of the cell cycle demonstrated an increase in the percentage of cells in the G2/M phase. The compounds caused apoptosis of the cells, mitochondrial depolarization, generation of reactive oxygen species, and activation of caspase-3, caspase-8, and caspase-9. Moreover, they acted as topoisomerase I inhibitors.

  14. The Partial Aminolysis of (NPF2)3 or 4.

    DTIC Science & Technology

    1978-12-01

    as (NPC1 2)3 ~ , with primary or secondary amines or with alkoxides or aryl - oxides have b:en studied in detail.2 Under suitable reaction conditions...reactions between II and n—butylamine carried out in the presence of lithium bromide gave products that were virtually identical to those fo rmed in...g, 0.006 ml) in 10 ml of TN! was added to a solution of sodium phenoxide (prepared from 11.04 g (0.48 aol) sodium and 58.7 g (0.62 aol) of phenol in

  15. 2-(4-Chloro-3,3,7-trimethyl-2,3-dihydro-1H-indol-2-yl-idene)-2-cyano-acetamide.

    PubMed

    Helliwell, Madeleine; Baradarani, Mehdi M; Alyari, Maryam; Afghan, Arash; Joule, John A

    2012-01-01

    Reaction of 2-(4-chloro-3,3,7-trimethyl-2,3-dihydro-1H-indol-2-yl-idene)propane-dial with hydroxyl-amine gives the title compound, C(14)H(14)ClN(3)O, in which the ring N atom is essentially planar [sum of angles around the ring N atom = 361°], indicating conjugation with the 2-cyano-acryl-amide unit. The orientation of the acetamide group arises from intra-molecular hydrogen bonding between the indole N-H and carbonyl groups. In the crystal, inversion-related acetamide groups form N-H⋯O hydrogen-bonded dimers in graph-set R(2) (2)(8) motifs, whilst dimers are also formed by pairs of amine-nitrile N-H⋯N hydrogen bonds in R(2) (2)(12) motifs. These inter-actions together generate ribbons that propagate along the b-axis direction.

  16. Luminescence and energy transfer properties of Sr3Y(PO4)3:Ce3+, Mn2+ phosphors

    NASA Astrophysics Data System (ADS)

    Lin, Jun; Hu, Yihua; Chen, Li; Wang, Zhonghua; Zhang, Shaoan

    2016-03-01

    A series of highly efficient Sr3-yY1-x(PO4)3:xCe3+,yMn2+(SYP:xCe3+, Mn2+) phosphors have been prepared via a solid state reaction. The XRD (X-ray diffraction) data, PL (photoluminescence) and PLE (photoluminescence excitation) properties and ET (energy transfer) mechanism of obtained phosphors were discussed. When prepared in air, the self-reducing process of turning Ce4+ into Ce3+ can be found in SYP:xCe3+ phosphor. A bright red light emission was presented in the Ce3+ and Mn2+ co-doping samples via the efficient ET from the sensitizer Ce3+ to Mn2+, which is ascribed to electric multipolar interaction between these two kinds of ions. The critical concentration of Ce3+ in SrY1-x(PO4)3:xCe3+ and Mn2+ in Sr3-yY1-x(PO4)3:xCe3+, yMn2+ are x=0.07 and y=0.15, respectively. In addition, the ET efficiency reach 51.6% when the luminescence intensity of Ce3+ is half of that in the absence of Mn2+ and the concentration of Mn2+ is 0.15. The emission color of the phosphors were also clarify by CIE coordinate briefly.

  17. The antinociceptive effect of 4-substituted derivatives of 5-(4-chlorophenyl)-2-(morpholin-4-ylmethyl)-2,4-dihydro-3H-1,2,4-triazole-3-thione in mice.

    PubMed

    Joanna, Listos; Talarek, Sylwia; Orzelska, Jolanta; Fidecka, Sylwia; Wujec, Monika; Plech, Tomasz

    2014-04-01

    The aim of the present experiments was to examine the antinociceptive activity of 4-substituted derivatives of 5-(4-chlorophenyl)-2-(morpholin-4-ylmethyl)-2,4-dihydro-3H-1,2,4-triazole-3-thione in mice. The compounds were synthesized using the so-called Mannich reaction and their structures were confirmed using IR and 1H-NMR spectra. The antinociceptive activity was investigated in two behavioral tests: the hot plate test and the writhing test. For preliminary estimation of other behavioral effects, the locomotor activity of mice, the motor coordination in the rota-rod test, and the myorelaxation in the chimney test were also studied. The changes in body temperature of animals were also recorded. We demonstrated that all examined compounds produced antinociceptive effect, both in the hot plate test and in the writhing test, without impact on the motor coordination and myorelaxation of animals. The pharmacological effect of all drugs has been developed within 60 min after administration of drugs; and in two cases (T-103 and T-104), it has been a short-lasting effect (up to 90 min). Two compounds (T-100 and T-102) also inhibited the locomotor activity of animals. T-104 induced the changes in body temperature of mice. Generally, we demonstrated that combination of two different heterocyclic systems (morpholine and 1,2,4-triazole) might be beneficial for reduction of nociception.

  18. Non-centrosymmetric Rb2Mn2(MoO4)3

    PubMed Central

    Bouzidi, Chahira; Zid, Mohamed Faouzi; Driss, Ahmed; Souilem, Amira

    2014-01-01

    The title compound, dirubidium dimanganese(II) tris­(tetra­oxo­molyb­date), Rb2Mn2(MoO4)3, was prepared by solid-state reactions. The structure can be described as being composed of MnO6 octa­hedra sharing corners with MoO4 tetra­hedra. The three-dimensional framework contains cavities in which the rubidium ions are located. The Rb+ cations are within distorted nine- and 12-vertex polyhedra. The pairs of different Mn2+ and Rb+ cations are each located on threefold rotation axes.. Rb2Mn2(MoO4)3 is isotypic with compounds of the Cs2 M 2Mo3O12 (M = Ni, Fe) family. A comparative structural description is provided between the structure of the title compound and those of related phases. Differences with structures such as alluaudite are discussed. PMID:25161508

  19. 1,1',4,5-tetrahydrotrispiro[1,3,2-diazaphosphole-2,2'-[1,3,5,2,4,6]triazatriphosphinine-4',6''-dibenzo[d,f][1,3,2]dioxaphosphepine-6',6'''-dibenzo[d,f][1,3,2]dioxaphosphepine

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The title compound 1,1',4,5-tetrahydrotrispiro[1,3,2-diazaphosphole-2,2'-[1,3,5,2,4,6]triazatriphosphinine-4',6''-dibenzo[d,f][1,3,2]dioxaphosphepine-6',6'''-dibenzo[d,f][1,3,2]dioxaphosphepine], C26H22N5O4P3, at 100°K has monoclinic (P21/c) symmetry and is achieved in a two step synthesis that does...

  20. Valence tautomerism of new pyrazolo[4,3-e]tetrazole[4,5-b][1,2,4]triazines

    NASA Astrophysics Data System (ADS)

    Mojzych, Mariusz; Karczmarzyk, Zbigniew; Wysocki, Waldemar; Urbańczyk-Lipkowska, Zofia; Żaczek, Natalia

    2014-06-01

    New pyrazolo[4,3-e]tetrazolo[4,5-b][1,2,4]triazines 5 and 6 were prepared as new biological active compounds with potential anticancer activity referring to our previous study. The 1H NMR spectra reveal tautomeric equilibrium azido and tricyclic forms of these compounds in solution. The molecular and crystal structures of 5 and 6 were determined by the X-ray analysis. The X-ray investigations show that in the crystalline state the compounds 5 and 6 exist as the linear tricyclic pyrazolo[4,3-e]tetrazolo[4,5-b][1,2,4]triazine tautomeric form. The analysis of the intra- and intermolecular interactions indicates the weak C-H⋯N hydrogen bonds and π⋯π interactions in crystal of 6 and van der Waals forces only in crystal of 5 as the non-covalent interactions influencing the molecular packing. The theoretical calculations at the ab initio DFT/B3LYP/6-311++G(d,p) level showed the azido form (3 and 4) as one existing in the gaseous phase and the coexistence of the tricyclic linear (5 and 6) and azido tautomeric forms in solution, wherein the contribution of the linear form compared to the azido form changes with polarity of the solvent.

  1. Blue and red long lasting phosphorescence (LLP) in β-Zn3(PO4)2:Mn2+,Zr4+

    NASA Astrophysics Data System (ADS)

    Wang, Jing; Su, Qiang; Wang, Shubin

    2005-07-01

    Multi-color long lasting phosphorescent (LLP) phenomenon in β-Zn3(PO4)2:Mn2+,Zr4+ was systematically investigated. It is found that the red (λEm=616 nm) LLP performance of Mn2+ such as brightness and duration is largely improved, and that the blue (λEm=475 nm) LLP of Zr4+ with lower intensity appears when Zr4+ ions are co-doped into the matrix. The fluorescence, phosphorescence and thermoluminescence (TL) spectra show that Mn2+ ion is solely expected as a luminescent center, while Zr4+ ion not only acts as a luminescent center, but also induces an electron trap (TrapZr) associated with a TL peak at 344 K. The trap depth for TrapZr is 0.25 eV, while that for the intrinsic trap is 0.38 eV, associated with a dominant peak at 385 K for Zn3(PO4)2:Mn2+. The Zr4+-induced trap with suitable depth is responsible for the improvement of the red LLP of Mn2+ ion and the appearance of the blue LLP of Zr4+ ion. The LLP mechanism is also investigated.

  2. (3R,4S)-3,4-Isopropyl­idenedioxy-3,4-dihydro-2H-pyrrole 1-oxide

    PubMed Central

    Flores, Mari Fe; Garcia, Pilar; M. Garrido, Narciso; Sanz, Francisca; Diez, David

    2011-01-01

    The title compound C7H11NO3 was prepared by intra­molecular nucleophilic displacement of 2,3-O-iso-propyl­idene-d-erythronolactol. There are two mol­ecules in the asymmetric unit, which are related by a pseudo-inversion centre. The crystal structure determination confirms unequivocally the configuration of the chiral centres as 3S,4R. In the crystal structure, inter­molecular C—H⋯O inter­actions link the mol­ecules (into infinite zigzag chains along the a axis. PMID:21754432

  3. Enantioselective synthesis and biological activity of (3S,4R)- and (3S,4S)-3-hydroxy-4-hydroxymethyl- 4-butanolides in relation to PGE2.

    PubMed

    Miranda, Pedro O; Estévez, Francisco; Quintana, José; García, Candelaria I; Brouard, Ignacio; Padrón, Juan I; Pivel, Juan P; Bermejo, Jaime

    2004-01-15

    Compounds 9 and 13 were synthesized, and their structures and stereochemistry were elucidated by spectroscopic methods. In competition binding experiments, specific [(3)H]-PGE(2) binding was significantly displaced by compound 9 and, to a lesser extent, by 13, in a dose-dependent manner. The biological properties of compound 9 were studied on HL-60 cells, and several effects were found related to those of PGE(2). Compound 9 increases c-fos mRNA level as does PGE(2) and antagonizes TPA-induced terminal differentiation.

  4. Docking and quantitative structure-activity relationship studies for 3-fluoro-4-(pyrrolo[2,1- f][1,2,4]triazin-4-yloxy)aniline, 3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)aniline, and 4-(4-amino-2-fluorophenoxy)-2-pyridinylamine derivatives as c-Met kinase inhibitors

    NASA Astrophysics Data System (ADS)

    Caballero, Julio; Quiliano, Miguel; Alzate-Morales, Jans H.; Zimic, Mirko; Deharo, Eric

    2011-04-01

    We have performed docking of 3-fluoro-4-(pyrrolo[2,1- f][1,2,4]triazin-4-yloxy)aniline (FPTA), 3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)aniline (FPPA), and 4-(4-amino-2-fluorophenoxy)-2-pyridinylamine (AFPP) derivatives complexed with c-Met kinase to study the orientations and preferred active conformations of these inhibitors. The study was conducted on a selected set of 103 compounds with variations both in structure and activity. Docking helped to analyze the molecular features which contribute to a high inhibitory activity for the studied compounds. In addition, the predicted biological activities of the c-Met kinase inhibitors, measured as IC50 values were obtained by using quantitative structure-activity relationship (QSAR) methods: Comparative molecular similarity analysis (CoMSIA) and multiple linear regression (MLR) with topological vectors. The best CoMSIA model included steric, electrostatic, hydrophobic, and hydrogen bond-donor fields; furthermore, we found a predictive model containing 2D-autocorrelation descriptors, GETAWAY descriptors (GETAWAY: Geometry, Topology and Atom-Weight AssemblY), fragment-based polar surface area (PSA), and MlogP. The statistical parameters: cross-validate correlation coefficient and the fitted correlation coefficient, validated the quality of the obtained predictive models for 76 compounds. Additionally, these models predicted adequately 25 compounds that were not included in the training set.

  5. Docking and quantitative structure-activity relationship studies for 3-fluoro-4-(pyrrolo[2,1-f][1,2,4]triazin-4-yloxy)aniline, 3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)aniline, and 4-(4-amino-2-fluorophenoxy)-2-pyridinylamine derivatives as c-Met kinase inhibitors.

    PubMed

    Caballero, Julio; Quiliano, Miguel; Alzate-Morales, Jans H; Zimic, Mirko; Deharo, Eric

    2011-04-01

    We have performed docking of 3-fluoro-4-(pyrrolo[2,1-f][1,2,4]triazin-4-yloxy)aniline (FPTA), 3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)aniline (FPPA), and 4-(4-amino-2-fluorophenoxy)-2-pyridinylamine (AFPP) derivatives complexed with c-Met kinase to study the orientations and preferred active conformations of these inhibitors. The study was conducted on a selected set of 103 compounds with variations both in structure and activity. Docking helped to analyze the molecular features which contribute to a high inhibitory activity for the studied compounds. In addition, the predicted biological activities of the c-Met kinase inhibitors, measured as IC(50) values were obtained by using quantitative structure-activity relationship (QSAR) methods: Comparative molecular similarity analysis (CoMSIA) and multiple linear regression (MLR) with topological vectors. The best CoMSIA model included steric, electrostatic, hydrophobic, and hydrogen bond-donor fields; furthermore, we found a predictive model containing 2D-autocorrelation descriptors, GETAWAY descriptors (GETAWAY: Geometry, Topology and Atom-Weight AssemblY), fragment-based polar surface area (PSA), and MlogP. The statistical parameters: cross-validate correlation coefficient and the fitted correlation coefficient, validated the quality of the obtained predictive models for 76 compounds. Additionally, these models predicted adequately 25 compounds that were not included in the training set.

  6. 2-Amino-4-(nitroalkyl)-4H-chromene-3-carbonitriles as New Cytotoxic Agents

    PubMed Central

    Zonouzi, Afsaneh; Mirzazadeh, Roghieh; Safavi, Maliheh; Kabudanian Ardestani, Sussan; Emami, Saeed; Foroumadi, Alireza

    2013-01-01

    A series of 2-amino-4-(nitroalkyl)-4H-chromene-3-carbonitriles were synthesized by an efficient multicomponent reaction in aqueous media using DBU as a catalyst at room temperature. Mild condition, environment friendly procedure and excellent yields are the main advantages of this procedure. The cytotoxic activity of target compounds were evaluated against three cancer cell lines MDA-MB-231, MCF-7 and T47D in comparison with etoposide as reference drug. Generally, all compounds showed good cell growth inhibitory activity with IC50 values less than 30 μg/mL. Their activities were comparable or more potent than standard drug etoposide. The 6-bromo- derivatives 7e and 7f showed promising cytotoxic activity with IC50 values in the range of 3.46–18.76 μg/mL, being more potent than etoposide against all tested cell lines. PMID:24523747

  7. 1,2,3,3′,4′,6′-Hexaacetyl-4,6-O-benzyl­idenesucrose

    PubMed Central

    Brito-Arias, Marco A.; Soto-Ortega, Miguel; García-Báez, Efrén V.

    2011-01-01

    In the title compound, C31H38O17, the 1,3-dioxane and pyran­oside rings both show 4 C 1 chair conformations while for the d-fructofuran­oside moiety an envelop 3E conformation is observed. The phenyl ring is oriented almost perpendicular to the 1,3-dioxane ring [dihedral angle = 79.3 (2)°], and the acetate groups are equatorial for the pyran­oside ring and axial for the furan­oside ring. The analysis of potential hydrogen bonds shows both intra- and inter­molecular C—H⋯O contacts to be present. PMID:21523142

  8. Synthesis and evaluation of the biological activities of some 3-{[5-(6-methyl-4-aryl-2-oxo-1,2,3,4-tetrahydropyrimidin-5-yl)-1,3,4-oxadiazol-2-yl]-imino}-1,3-dihydro-2H-indol-2-one derivatives.

    PubMed

    George, Sonia; Parameswaran, Manoj Kumar; Chakraborty, Acharjee Raja; Ravi, Thengungal Kochupappy

    2008-03-01

    Reaction of ethyl-6-methyl-2-oxo-4-aryl-1,2,3,4-tetrahydropyrimidin-5-carboxylates (1a-i) with hydrazine hydrate yielded 6-methyl-2-oxo-4-aryl-1,2,3,4-tetrahydropyrimidin-5-carbohydrazides (2a-i). These products, on reaction with cyanogen bromide, gave 5-(5-amino-1,3,4-oxadiazol-2-yl)-6-methyl-4-aryl-3,4-dihydropyrimidin-2 (1H)-ones (3a-i). The resultant aminooxadiazolylpyrimidinones were condensed with isatin to obtain various 3-{[5-(6-methyl-4-aryl-2-oxo-1,2,3,4-tetrahydropyrimidin-5-yl)-1,3,4-oxadiazol-2-yl]-imino}-1,3-dihydro-2H-indol-2-ones (4a-i). These products were characterized by IR, 1H NMR, mass spectra and elemental analysis. Products (4a-i) revealed promising antibacterial, antifungal and antioxidant activity.

  9. Redetermination of brackebuschite, Pb2Mn3+(VO4)2(OH)

    PubMed Central

    Lafuente, Barbara; Downs, Robert T.

    2016-01-01

    The crystal structure of brackebuschite, ideally Pb2Mn3+(VO4)2(OH) [dilead(II) manganese(III) vanadate(V) hydroxide], was redetermined based on single-crystal X-ray diffraction data of a natural sample from the type locality Sierra de Cordoba, Argentina. Improving on previous results, anisotropic displacement parameters for all non-H atoms were refined and the H atom located, obtaining a significant improvement of accuracy and an unambiguous hydrogen-bonding scheme. Brackebuschite belongs to the brackebuschite group of minerals with general formula A 2 M(T1O4)(T2O4)(OH, H2O), with A = Pb2+, Ba, Ca, Sr; M = Cu2+, Zn, Fe2+, Fe3+, Mn3+, Al; T1 = As5+, P, V5+; and T2 = As5+, P, V5+, S6+. The crystal structure of brackebuschite is based on a cubic closest-packed array of O and Pb atoms with infinite chains of edge-sharing [Mn3+O6] octa­hedra located about inversion centres and decorated by two unique VO4 tetra­hedra (each located on a special position 2e, site symmetry m). One type of VO4 tetra­hedra is linked with the 1 ∞[MnO4/2O2/1] chain by one common vertex, alternating with H atoms along the chain, while the other type of VO4 tetra­hedra link two adjacent octa­hedra by sharing two vertices with them and thereby participating in the formation of a three-membered Mn2V ring between the central atoms. The 1 ∞[Mn3+(VO4)2OH] chains run parallel to [010] and are held together by two types of irregular [PbOx] polyhedra (x = 8, 11), both located on special position 2e (site symmetry m). The magnitude of the libration component of the O atoms of the 1 ∞[Mn3+(VO4)2OH] chain increases linearly with the distance from the centerline of the chain, indicating a significant twisting to and fro of the chain along [010]. The hy­droxy group bridges one Pb2+ cation with two Mn3+ cations and forms an almost linear hydrogen bond with a vanadate group of a neighbouring chain. The O⋯O distance of this inter­action determined from the structure refinement agrees well with

  10. Redetermination of brackebuschite, Pb2Mn(3+)(VO4)2(OH).

    PubMed

    Lafuente, Barbara; Downs, Robert T

    2016-03-01

    The crystal structure of brackebuschite, ideally Pb2Mn(3+)(VO4)2(OH) [dilead(II) manganese(III) vanadate(V) hydroxide], was redetermined based on single-crystal X-ray diffraction data of a natural sample from the type locality Sierra de Cordoba, Argentina. Improving on previous results, anisotropic displacement parameters for all non-H atoms were refined and the H atom located, obtaining a significant improvement of accuracy and an unambiguous hydrogen-bonding scheme. Brackebuschite belongs to the brackebuschite group of minerals with general formula A 2 M(T1O4)(T2O4)(OH, H2O), with A = Pb(2+), Ba, Ca, Sr; M = Cu(2+), Zn, Fe(2+), Fe(3+), Mn(3+), Al; T1 = As(5+), P, V(5+); and T2 = As(5+), P, V(5+), S(6+). The crystal structure of brackebuschite is based on a cubic closest-packed array of O and Pb atoms with infinite chains of edge-sharing [Mn(3+)O6] octa-hedra located about inversion centres and decorated by two unique VO4 tetra-hedra (each located on a special position 2e, site symmetry m). One type of VO4 tetra-hedra is linked with the (1) ∞[MnO4/2O2/1] chain by one common vertex, alternating with H atoms along the chain, while the other type of VO4 tetra-hedra link two adjacent octa-hedra by sharing two vertices with them and thereby participating in the formation of a three-membered Mn2V ring between the central atoms. The (1) ∞[Mn(3+)(VO4)2OH] chains run parallel to [010] and are held together by two types of irregular [PbO x ] polyhedra (x = 8, 11), both located on special position 2e (site symmetry m). The magnitude of the libration component of the O atoms of the (1) ∞[Mn(3+)(VO4)2OH] chain increases linearly with the distance from the centerline of the chain, indicating a significant twisting to and fro of the chain along [010]. The hy-droxy group bridges one Pb(2+) cation with two Mn(3+) cations and forms an almost linear hydrogen bond with a vanadate group of a neighbouring chain. The O⋯O distance of this inter-action determined from the

  11. Synthesis, crystal structure, and thermal studies of (NH 4) 2Cd 2(SeO 4) 3·3H 2O

    NASA Astrophysics Data System (ADS)

    Martínez, M. L.; Rodriguez, A.; Mestres, L.; Solans, X.; Bocanegra, E. H.

    1990-11-01

    The species (NH 4) 2Cd 2(SeO 4) 3.3H 2O has been synthesized and its crystal structure has been determined. Crystals were obtained by slow evaporation from an aqueous solution at 85-90°C. The compound is monoclinic, {P2 1}/{m}, a = 6.836(2), b = 19.372(4), c = 5.690(2) Å, β = 94.02(2)°, V = 751.7(6) Å 3, Dx = 3.285 g cm -3, Z = 2; F(000) = 692.0, λ(Mo Kα) = 0.71069Å, μ(Mo Kα) = 106.99 cm -1, 298 K. Refinement was terminated at R = 0.043 for all observed reflections. Two kinds of tetrahedrally coordinated selenium atoms occur in the structure which form double chains which in turn give the three-dimensional structure. The cadmium atoms are coordinated by five oxygen atoms from different selenate anions, and by an oxygen atom from a water molecule. This structure gives cavities, each one accommodating a water molecule and two ammonium groups. Thermogravimetry shows that the anhydrous species of langbeinite stoichiometry is not stable.

  12. High Temperature Transfer Molding Resins Based on 2,3,3',4'-Biphenyltetracarboxylic Dianhydride

    NASA Technical Reports Server (NTRS)

    Smith, J. G., Jr.; Connell, J. W.; Hergenrother, P. M.; Yokota, R.; Criss, J. M.

    2002-01-01

    As part of an ongoing effort to develop materials for resin transfer molding (RTM) processes to fabricate high performance/high temperature composite structures, phenylethynyl containing imides have been under investigation. New phenylethynyl containing imide compositions were prepared using 2,3,3',4'-biphenyltetracarboxylic dianhydride (a-BPDA) and evaluated for cured glass transition temperature (Tg), melt flow behavior, and for processability into flat composite panels via RTM. The a-BPDA imparts a unique combination of properties that are desirable for high temperature transfer molding resins. In comparison to its symmetrical counterpart (i.e. 3,3',4,4'-biphenyltetracarboxylic dianhydride), a-BPDA affords oligomers with lower melt viscosities and when cured, higher Tgs. Several candidates exhibited the appropriate combination of properties such as a low and stable melt viscosity required for RTM processes, high cured Tg, and moderate toughness. The chemistry, physical, and composite properties of select resins will be discussed.

  13. 2,3-trans-3,4-trans-3,4-Dihydroxy-L-proline: An amino acid in toxic peptides of Amanita virosa mushrooms

    PubMed Central

    Buku, A.; Faulstich, H.; Wieland, T.; Dabrowski, J.

    1980-01-01

    Among the four possible stereoisomers of 3,4-dihydroxy-L-proline,2,3-trans-3,4-trans-3,4-dihydroxy-L-proline (IV) had not been found in nature previously. It has now been detected as a component of virotoxins, toxic peptides of Amanita virosa mushrooms. Because periodate failed to effect an oxidative glycol splitting reaction, the two hydroxyl groups in positions 3 and 4 were expected to be in a trans configuration. Furthermore, the formation of a 4-lactone on treatment with acids pointed to the carboxyl group and the hydroxyl group at position 4 being in a cis configuration. These results are in agreement with structure IV only. Final proof for structure IV was given by NMR spectroscopy and direct comparison with the 2,3-cis-3,4-trans-3,4-dihydroxy-L-proline isomer. PMID:16592813

  14. Metastability in the MgAl2O4-Al2O3 System

    DOE PAGES

    Wilkerson, Kelley R.; Smith, Jeffrey D.; Hemrick, James G.

    2014-07-22

    Aluminum oxide must take a spinel form ( γ-Al2O3) at elevated temperatures in order for extensive solid solution to form between MgAl2O4 and α-Al2O3. The solvus line between MgAl2O4 and Al2O3 has been defined at 79.6 wt% Al2O3 at 1500°C, 83.0 wt% Al2O3 at 1600°C, and 86.5 wt% Al2O3 at 1700°C. A metastable region has been defined at temperatures up to 1700°C which could have significant implications for material processing and properties. Additionally, initial processing could have major implications on final chemistry. The spinel solid solution region has been extended to form an infinite solid solution with Al2O3 at elevatedmore » temperatures. A minimum in melting at 1975°C and a chemistry of 96 wt% Al2O3 rather than a eutectic is present, resulting in no eutectic crystal formation during solidification.« less

  15. High-temperature deformation and microstructural analysis for Si3N4-Sc2O3

    NASA Technical Reports Server (NTRS)

    Cheong, Deock-Soo; Sanders, William A.

    1990-01-01

    It was indicated that Si3N4 doped with Sc2O3 may exhibit high temperature mechanical properties superior to Si3N4 systems with various other oxide sintered additives. High temperature deformation of samples was studied by characterizing the microstructures before and after deformation. It was found that elements of the additive, such as Sc and O, exist in small amounts at very thin grain boundary layers and most of them stay in secondary phases at triple and multiple grain boundary junctions. These secondary phases are devitrified as crystalline Sc2Si2O7. Deformation of the samples was dominated by cavitational processes rather than movements of dislocations. Thus the excellent deformation resistance of the samples at high temperature can be attributed to the very small thickness of the grain boundary layers and the crystalline secondary phase.

  16. Condensed imidazo-1,2,4-azines. 15. Reaction of 1,2-diaminobenzimidazole with 5-phenyl-2,3-dihydrofuran-2,3-dione

    SciTech Connect

    Kruglenko, V.P.; Gnidets, V.P.; Klyuev, N.A.; Povstyanoi, M.V.

    1987-10-01

    The reaction of 1,2-diaminobenzimidazole with 5-phenyl-2,3-dihydrofuran-2,3-dione in acetic acid gave a mixture of 2-benzoylmethyl-1,2,4-triazino (2,3-..cap alpha..)-benzimidazol-4H-3-one and 3-benzoylmethyl-1,2,4-triazino(2,3-..cap alpha..)benzimidazol-1H-2-one, the intramolecular cyclization of which gave isomeric 2-phenylfuro-(5,4-e)- and 2-phenylfuro(4,5-e)-1,2,4-triazino(2,3-..cap alpha..)benzimidazoles. Only the corresponding furo(4,5-e)-1,2,4-triazino(2,3-..cap alpha..)benzimidazole was isolated when the reaction was carried out in sulfuric acid. The IR spectra of KBr pellets of the compounds were recorded with a UR-20 spectrometer. The electronic absorption spectra of solutions in dioxane were obtained with a Specord UV-vis spectrophotometer. The mass spectra were recorded with a Varian MAT-311a spectrometer. The quantum-chemical calculations were made by the Pariser-Parr-Pople (PPP) method with the standard parametrization.

  17. Failure to induce mutations in Chinese hamster V79 cells and WB rat liver cells by the polybrominated biphenyls, Firemaster BP-6, 2,2',4,4',5,5'-hexabromobiphenyl, 3,3',4,4',5,5'-hexabromobiphenyl, and 3,3',4,4'-tetrabromobiphenyl.

    PubMed

    Kavanagh, T J; Rubinstein, C; Liu, P L; Chang, C C; Trosko, J E; Sleight, S D

    1985-06-15

    Firemaster BP-6 (FM), a mixture of polybrominated biphenyls (PBB), and the congeners 2,2',4,4',5,5'-hexabromobiphenyl (2,4,5-HBB), 3,3',4,4',5,5'-hexabromobiphenyl (3,4,5-HBB), and 3,3',4,4'-tetrabromobiphenyl (3,4-TBB) were tested for their ability to induce mutations in mammalian cells in culture. A rat liver microsome-mediated (S 15) Chinese hamster V79 cell mutation assay was used to test the mutagenicity of PBB and 3,4-TBB. V79 cells and WB rat liver cells were used to detect the mutagenicity of 2,4,5-HBB and 3,4,5-HBB. No mutagenic effects were detected at the dose levels tested. The possibility that these compounds promote liver neoplasms via a nongenotoxic mechanism is discussed.

  18. Platelet activating factor antagonist design: structure of methyl trans-5-(3,4-dimethoxyphenyl)-2,3,4,5-tetrahydro-2-oxo-4- furancarboxylate.

    PubMed

    Peterson, J R; Smillie, T J; Rogers, R D

    1989-02-15

    C14H16O6, Mr = 280.28, monoclinic, P2(1)/c, a = 6.070 (2), b = 9.526 (5), c = 22.418 (5) A, beta = 94.32 (2) degrees, V = 1293 A3, Z = 4, Dx = 1.44 g cm-3, lambda(Mo K alpha) = 0.71073 A, mu = 0.71 cm-1, F(000) = 592, T = 293 K, final R = 0.043 for 1400 observed [F0 greater than or equal to 5 sigma(F0)] reflections. The observed structure confirms a trans stereorelationship for the two substituents and an envelope conformation for the lactone ring. There is no crystallographically imposed symmetry. An analysis of the closest contacts in the cell lattice reveals two types of intermolecular interactions for this compound.

  19. Investigation of the association behaviors between bovine serum albumin and 2-(4-methylphenyl)-3-(N-acetyl)-5-(2,4-dichlorophenoxymethyl)-1,3,4-oxodiazoline.

    PubMed

    Huang, Zhenzhong; Wang, Ruiling; Han, Erwei; Xu, Lifan; Song, Yonghai

    2013-07-01

    The study was designed to examine the interaction between 2-(4-methylphenyl)-3-(N-acetyl)-5-(2,4-dichlorophenoxymethyl)-1,3,4-oxodiazoline (MPNDO) and bovine serum albumin (BSA) under physiological conditions by using fluorescence spectroscopy, ultraviolet absorption spectroscopy, FT-IR spectroscopy and circular dichroism spectroscopy and atomic force microscope. Spectroscopic analysis of the fluorescence emission quenching and ultraviolet absorption revealed that the quenching mechanism of bovine serum albumin by MPNDO was static quenching procedure. The binding constant and binding sites number at different temperatures were measured. The average binding distances between donor (BSA) and acceptor (MPNDO) was estimated to be 1.46 nm (301 K), based on the Föster non-radioactive energy transfer theory. An average size of 3.1 nm had a high proportion and these dots might be ascribed to BSA, some other dots with an average size of 6.6 nm might result from BSA-MPNDO bioconjugates while the average diameter of MPNDO was 1.6 nm, which was reasonable to conclude that one BSA-MPNDO bioconjugates consisted of one BSA and one MPNDO. The thermodynamic parameters, enthalpy change (ΔH), entropy change (ΔS) and free energy change (ΔG) were calculated, which indicated that the action force was mainly van der Waals forces. The data collected through synchronous fluorescence, FT-IR spectroscopy and circular dichroism spectroscopy demonstrated that the conformation of BSA was not affected obviously in the presence of MPNDO.

  20. Crystal structure of 4,4',4''-(1,3,5-triazine-2,4,6-tri-yl)tripyridinium trichloride 2.5-hydrate.

    PubMed

    Ling, Bo-Kai; Feng, Xiao-Long; Li, Yang; Luan, Tian-Gang

    2015-11-01

    The asymmetric unit of the title compound, C18H15N6 (3+)·3Cl(-)·2.5H2O, contains two independent (1,3,5-triazine-2,4,6-tri-yl)tripyridinium cations. Both cations are approximately planar, the r.m.s. deviations of fitted non-H atoms being 0.045 and 0.051 Å. In the crystal, extensive O-H⋯Cl, O-H⋯O, N-H⋯Cl and N-H⋯O hydrogen bonds and weak C-H⋯Cl and C-H⋯O inter-actions link the organic cations, Cl(-) anions and water mol-ecules into a three-dimensional supra-molecular architecture. π-π stacking between the pyridine rings of adjacent cations is also observed, the centroid-to-centroid distance being 3.7578 (8) Å.

  1. Pressure-enhanced superconductivity in Eu3Bi2S4F4

    DOE PAGES

    Luo, Yongkang; Zhai, Hui -Fei; Zhang, Pan; ...

    2014-12-17

    The pressure effect on the newly discovered charge-transferred BiS2-based superconductor, Eu3Bi2S4F4, with a Tc of 1.5 K at ambient pressure, is investigated by transport and magnetic measurements. Accompanied with the enhancement of metallicity under pressures, the onset superconducting transition temperature increases abruptly around 1.0 GPa, reaching ~10.0 K at 2.26 GPa. Alternating current magnetic susceptibility measurements indicate that a new superconducting phase with a higher Tc emerges and dominates at high pressures. In the broad pressure window of 0.68GPa≤p≤2.00 GPa, the high-Tc phase coexists with the low-Tc phase. Hall effect measurements reveal a significant difference in electronic structures between themore » two superconducting phases. As a result, our work devotes the effort to establish the commonality of pressure effect on the BiS2-based superconductors, and also uncovers the importance of electron carrier density in the high-Tc phase.« less

  2. Electron impact mass spectral fragmentation of 3a,5-disubstituted 1, 3-diphenyl-3a,4,5,6-tetra-hydro-3H-1,2,4-triazolo[4,3-a][1, 5]benzo-diazepines.

    PubMed

    Xu, J; Zhang, Q; Wang, C

    2000-01-01

    The mass spectrometric behaviour of six 3a,5-disubstituted 1, 3-diphenyl-3a,4,5,6-tetrahydro-3H-1,2,4-triazolo[4,3-a][1, 5]benzodiazepines has been studied with the aid of mass-analyzed ion kinetic energy spectrometry and accurate mass measurements under electron impact ionization. All compounds show a tendency to eliminate (substituted) styrene molecules, aryl radicals, arylmethyl radicals or phenylnitrene (PhN:). All of the resulting fragment ions, except [M - PhN:](+.), could further undergo a reverse [2 + 3] cycloaddition. The [M - PhN:](+.) ions could further lose styrene derivatives and undergo a ring enlargement rearrangement. The molecular ions also show a tendency to eliminate a phenyl radical, and the [M - Ph](+) ions could eliminate styrene derivatives. The [M - R(1)CH = CH(2)](+.) ions could further lose NH(2) to yield stable tetracyclic 1,3-diphenyl-1,2,4-triazolo[4,3-d]phenanthridine ions, which could further lose benzonitrile, or undergo a reverse [2 + 3] cycloaddition. The molecular ions could also undergo a reverse [2 + 3] cycloaddition to produce N-phenylbenzonitrile imine ions and 2, 4-disubstituted 2,3-dihydro-1H-1,5-benzodiazepine ions, whose further fragmentations were also investigated.

  3. Isotope shift of 40,42,44,48Ca in the 4s 2S1/24p 2P3/2 transition

    NASA Astrophysics Data System (ADS)

    Gorges, C.; Blaum, K.; Frömmgen, N.; Geppert, Ch; Hammen, M.; Kaufmann, S.; Krämer, J.; Krieger, A.; Neugart, R.; Sánchez, R.; Nörtershäuser, W.

    2015-12-01

    We report on improved isotope shift measurements of the isotopes {}{40,42,{44,48}}Ca in the 4{{s}}{ }2{{{S}}}1/2\\to 4{{p}}{ }2{{{P}}}3/2 (D2) transition using collinear laser spectroscopy. Accurately known isotope shifts in the 4{{s}}{ }2{{{S}}}1/2\\to 4{{p}}{ }2{{{P}}}1/2(D1) transition were used to calibrate the ion beam energy with an uncertainty of {{Δ }}U≈ +/- 0.25 {{V}}. The accuracy in the D2 transition was improved by a factor of 5-10. A King-plot analysis of the two transitions revealed that the field shift factor in the D2 line is about 1.8(13)% larger than in the D1 transition which is ascribed to relativistic contributions of the 4{{{p}}}1/2 wave function.

  4. 1-(6-Bromo-3,4-dihydro-2H-1,4-benz­oxazin-4-yl)-2,2-dichloro­ethanone

    PubMed Central

    Ye, Fei; Li, Ying; Fu, Ying; Zhao, Li-Xia; Gao, Shuang

    2012-01-01

    The title compound, C10H8BrCl2NO2, is a target mol­ecule in our research on herbicide safeners. The oxazine ring has an envelope conformation, with puckering parameters close to ideal values [Q = 0.498 (3) Å, θ = 53.7 (3)° and ϕ = 253.4 (4)°]. The crystal structure is stabilized by C—H⋯O, C—H⋯Cl and C—H⋯Br inter­actions. PMID:22904947

  5. 1-(6-Bromo-3,4-dihydro-2H-1,4-benz-oxazin-4-yl)-2,2-dichloro-ethanone.

    PubMed

    Ye, Fei; Li, Ying; Fu, Ying; Zhao, Li-Xia; Gao, Shuang

    2012-08-01

    The title compound, C(10)H(8)BrCl(2)NO(2), is a target mol-ecule in our research on herbicide safeners. The oxazine ring has an envelope conformation, with puckering parameters close to ideal values [Q = 0.498 (3) Å, θ = 53.7 (3)° and ϕ = 253.4 (4)°]. The crystal structure is stabilized by C-H⋯O, C-H⋯Cl and C-H⋯Br inter-actions.

  6. (Z)-5-(3,4,5-Tri-meth-oxy-styr-yl)-2,3-di-hydro-thieno[3,4-b][1,4]dioxine.

    PubMed

    Liu, Yu-Tao; Chu, Gang

    2014-04-01

    In the title compound, C17H18O5S, an analogue of the potent anti-cancer agent combretastatin A-4, the alkene C=C bond has a cis conformation and the C-C=C-C torsion angle is 9.0 (3)°. The dihedral angle between the benzene and thio-phene rings is 54.07 (4)°. The dioxene ring adopts a half-chair conformation, with the C atoms of the methyl-ene groups displaced by -0.325 (2) and 0.341 (3) Å from the plane of the other atoms. The C atoms of the two meta-meth-oxy groups are close to being coplanar with their attached benzene ring [displacements = -0.025 (2) and -0.196 (2) Å], whereas the C atom of the para-meth-oxy group is significantly displaced [by -1.107 (2) Å]. In the crystal, C-H⋯O hydrogen bonds link the mol-ecules into [0-11] chains, which feature two different types of R 2 (2)(6) loops.

  7. Thermodynamic Properties of α-Fe2O3 and Fe3O4 Nanoparticles

    DOE PAGES

    Spencer, Elinor C.; Ross, Nancy L.; Olsen, Rebecca E.; ...

    2015-04-21

    Here we comprehansively assessed the thermodynamic properties of hydrated α-Fe2O3 (hematite) and Fe3O4 (magnetite) nanoparticles. In addition to 9 nm Fe3O4, three α-e2O3nanoparticles samples of different sizes (11, 14, and 25 nm) and bulk α-e2O3 have been evaluated by inelastic neutron scattering methods. The contribution of the two-level magnetic spin flip transition to the heat capacity of the α-e2O3 particles has been determined. The isochoric heat capacity of the water confined on the surface of these two types of iron oxide particles have been calculated from their INS spectra, and is affected by the chemical composition of the underlying particle.more » Furthermore, the heat capacity and dynamics of the particle hydration layers appear to be influenced by a complex array of factors including particle size, water coverage, and possibly the magnetic state of the particle itself.« less

  8. Histone H3R2 symmetric dimethylation and histone H3K4 trimethylation are tightly correlated in eukaryotic genomes

    PubMed Central

    Yuan, Chih-Chi; Matthews, Adam G.W.; Jin, Yi; Chen, Chang Feng; Chapman, Brad A.; Ohsumi, Toshiro K.; Glass, Karen C.; Kutateladze, Tatiana G.; Borowsky, Mark L.; Struhl, Kevin; Oettinger, Marjorie A.

    2012-01-01

    Summary The preferential in vitro interaction of the PHD finger of RAG2, a subunit of the V(D)J recombinase, with histone H3 tails simultaneously trimethylated at lysine 4 and symmetrically dimethylated at arginine 2 (H3R2me2sK4me3) predicted the existence of the previously unknown histone modification, H3R2me2s. Here, we report the in vivo identification of H3R2me2s . Consistent with the binding specificity of the RAG2 PHD finger, high levels of H3R2me2sK4me3 are found at antigen receptor gene segments ready for rearrangement. However, this double modification is much more general; it is conserved throughout eukaryotic evolution. In mouse, H3R2me2s is tightly correlated with H3K4me3 at active promoters throughout the genome. Mutational analysis in S. cerevisiae reveals that deposition of H3R2me2s requires the same Set1 complex that deposits H3K4me3. Our work suggests that H3R2me2sK4me3, not simply H3K4me3 alone, is the mark of active promoters, and that factors that recognize H3K4me3 will have their binding modulated by their preference for H3R2me2s. PMID:22720264

  9. Sintering, properties and fabrication of Si3N4 + Y2O3 based ceramics

    NASA Technical Reports Server (NTRS)

    Quackenbush, C. L.; Smith, J. T.; Neil, J. T.; French, K. W.

    1983-01-01

    Pure silicon nitride shows a remarkable resistance to sintering without the use of densification additives. The present investigation is concerned with results which show the effect of chemical content on sinterability, taking into account the composition, raw material impurities, and processing contaminants. Aspects of sintering are discussed along with strength characteristics, and oxidation relations. Attention is given to phase field I and II materials, phase field III and IV materials, tungsten carbide and oxidation at 600 C, and studies involving shape fabrication by injection molding. It was found that in sintering Si3N4 + Y2O3 an increase in the amount of Y2O3 and, in particular, the addition of Al2O3 enhances the fluidity of the liquid phase.

  10. Monolithic thermally bonded Er3+, Yb3+:glass/Co2+:MgAl2O4 microchip lasers

    NASA Astrophysics Data System (ADS)

    Mlynczak, Jaroslaw; Belghachem, Nabil

    2015-12-01

    The highest ever reported 10 kW peak power in monolithic thermally bonded Er3+, Yb3+:glass/Co2+:MgAl2O4 microchip laser was achieved. To show the superiority of monolithic microchip lasers over those with external mirrors the laser generation characteristics of the same samples in both cases were compared.

  11. Antihypertensive activity of 2[(2-hydroxyphenyl)amino]-4(3H)-quinazolinone.

    PubMed

    Hussain, M A; Chiu, A T; Price, W A; Timmermans, P B; Shefter, E

    1988-04-01

    Two 2-substituted 4(3H)-quinazolinones were synthesized through an easy one-step synthetic procedure. One of them (1), which was synthesized by the reaction of 1-(2-hydroxyphenyl)-2-thiourea and isatoic anhydride, contained a guanidino moiety and showed antihypertensive activity following cumulative intravenous administration to anesthetized spontaneously hypertensive rats. The other compound (2) does not contain the guanidino group and did not exhibit antihypertensive activity.

  12. Refined Synthesis of 2,3,4,5-Tetrahydro-1,3,3-trimethyldipyrrin, a Deceptively Simple Precursor to Hydroporphyrins

    PubMed Central

    Ptaszek, Marcin; Bhaumik, Jayeeta; Kim, Han-Je; Taniguchi, Masahiko; Lindsey, Jonathan S.

    2008-01-01

    2,3,4,5-Tetrahydro-1,3,3-trimethyldipyrrin (1) is a crucial building block in the rational synthesis of chlorins and oxochlorins. The prior 5-step synthesis of 1 from pyrrole-2-carboxaldehyde (2) employed relatively simple and well-known reactions yet suffered from several drawbacks, including limited scale (≥ 0.5 g of 1 per run). A streamlined preparation of 1 has been developed that entails four steps: (i) nitro-aldol condensation of 2 and nitromethane under neat conditions to give 2-(2-nitrovinyl)pyrrole (3), (ii) reduction of 3 with NaBH4 to give 2-(2-nitroethyl)pyrrole (4), (iii) Michael addition of 4 with mesityl oxide under neat conditions or at high concentration to give γ-nitrohexanonepyrrole 5, and (iv) reductive cyclization of 5 with zinc/ammonium formate to give 1. Several multistep transformations have been established, including the direct conversion of 2 → 1. The advantages of the new procedures include (1) fewer steps, (2) avoidance of several problematic reagents, (3) diminished consumption of solvents and reagents, (4) lessened reliance on chromatography, and (5) scalability. The new procedures facilitate the preparation of 1 at the multigram scale. PMID:19132135

  13. Synthesis of 2-azaspiro[4.4]nonan-1-ones via phosphine-catalysed [3+2]-cycloadditions

    SciTech Connect

    Yong, Sarah R.; Williams, Morwenna C.; Pyne, Stephen G.; Ung, Alison T.; Skelton, Brian W.; White, Allan H.; Turner, Peter

    2008-10-03

    The phosphine-catalyzed [3+2]-cycloaddition of the 2-methylene {gamma}-lactams 4 and 5 and the acrylate 6 with the ylides derived from the ethyl ester, the amide or the chiral camphor sultam derivative of 2-butynoic acid (7a-c) give directly, or indirectly after reductive cyclization, spiro-heterocyclic products. The acid 32 underwent Curtius rearrangement and then acid hydrolysis to give two novel spiro-cyclic ketones, 41 and 42.

  14. 3' Phosphatase activity toward phosphatidylinositol 3,4-bisphosphate [PI(3,4)P2] by voltage-sensing phosphatase (VSP).

    PubMed

    Kurokawa, Tatsuki; Takasuga, Shunsuke; Sakata, Souhei; Yamaguchi, Shinji; Horie, Shigeo; Homma, Koichi J; Sasaki, Takehiko; Okamura, Yasushi

    2012-06-19

    Voltage-sensing phosphatases (VSPs) consist of a voltage-sensor domain and a cytoplasmic region with remarkable sequence similarity to phosphatase and tensin homolog deleted on chromosome 10 (PTEN), a tumor suppressor phosphatase. VSPs dephosphorylate the 5' position of the inositol ring of both phosphatidylinositol 3,4,5-trisphosphate [PI(3,4,5)P(3)] and phosphatidylinositol 4,5-bisphosphate [PI(4,5)P(2)] upon voltage depolarization. However, it is unclear whether VSPs also have 3' phosphatase activity. To gain insights into this question, we performed in vitro assays of phosphatase activities of Ciona intestinalis VSP (Ci-VSP) and transmembrane phosphatase with tensin homology (TPTE) and PTEN homologous inositol lipid phosphatase (TPIP; one human ortholog of VSP) with radiolabeled PI(3,4,5)P(3). TLC assay showed that the 3' phosphate of PI(3,4,5)P(3) was not dephosphorylated, whereas that of phosphatidylinositol 3,4-bisphosphate [PI(3,4)P(2)] was removed by VSPs. Monitoring of PI(3,4)P(2) levels with the pleckstrin homology (PH) domain from tandem PH domain-containing protein (TAPP1) fused with GFP (PH(TAPP1)-GFP) by confocal microscopy in amphibian oocytes showed an increase of fluorescence intensity during depolarization to 0 mV, consistent with 5' phosphatase activity of VSP toward PI(3,4,5)P(3). However, depolarization to 60 mV showed a transient increase of GFP fluorescence followed by a decrease, indicating that, after PI(3,4,5)P(3) is dephosphorylated at the 5' position, PI(3,4)P(2) is then dephosphorylated at the 3' position. These results suggest that substrate specificity of the VSP changes with membrane potential.

  15. Synthesis and antifungal activity of 2H-1,4-benzoxazin-3(4H)-one derivatives.

    PubMed

    Śmist, Małgorzata; Kwiecień, Halina; Krawczyk, Maria

    2016-01-01

    A series of 2-alkyl-2H-1,4-benzoxazin-3(4H)-ones (4a-l) was easily synthesized by two-step process involving O-alkylation of 2-nitrophenols with methyl 2-bromoalkanoates and next "green" catalytic reductive cyclization of the obtained 2-nitro ester intermediates (3a-l). Further, 6,7-dibromo (5a-c) and N-acetyl (6) derivatives were prepared by bromination and acetylation of unsubstituted 2-alkyl-2H-1,4-benzoxazin-3(4H)-ones (4a-c). The novel compounds (3a-l, 4d-l, 5a-c and 6) were fully characterized by spectroscopic methods (MS, (1)H and (13)C NMR). 2-Alkyl-2H-1,4-benzoxazin-3(4H)-ones (4a-l, 5a-c and 6) were screened for antifungal activity. Preliminary assays were performed using two methods: in vitro against seven phytopathogenic fungi-Botrytis cinerea, Phythophtora cactorum, Rhizoctonia solani, Phoma betae, Fusarium culmorum, Fusarium oxysporum and Alternaria alternata-and in vivo against barley powdery mildew Blumeria graminis. The tested compounds displayed moderate to good antifungal activity at high concentration (200 mg L(-1)). The most potent compounds were 2-ethyl-2H-1,4-benzoxazin-3(4H)-one (4a), 2-ethyl-7-fluoro-2H-1,4-benzoxazin-3(4H)-one (4g) and 4-acetyl-2-ethyl-2H-1,4-benzoxazin-3(4H)-one (6), which completely inhibited the mycelial growth of seven agricultural fungi at the concentration of 200 mg L(-1) in the in vitro tests. Moreover, 2-ethyl-2H-1,4-benzoxazin-3(4H)-one (4a) and 4-acetyl-2-ethyl-2H-1,4-benzoxazin-3(4H)-one (6) were also screened for antifungal activity at concentrations of 100 mg L(-1) and 20 mg L(-1). In the concentration of 100 mg L(-1), the N-acetyl derivative (6) completely inhibited the growth of three strains of fungi (F. culmorum, P. cactorum and R. solani), while 2-ethyl-2H-1,4-benzoxazin-3(4H)-one (4a) completely inhibited only R. solani strain. At the concentration of 20 mg L(-1), compound 6 showed good activity only against P. cactorum strain (72%).

  16. Reactions of phthalazine, quinazoline, 4,7-phenanthroline and 2,3'-bipyridine with ruthenium carbonyl.

    PubMed

    Cabeza, Javier A; Pruneda, Vanessa

    2012-06-28

    The reactions of [Ru(3)(CO)(12)] with four aromatic diazines have been studied in THF at reflux temperature. With phthalazine (L(1)), the compound [Ru(3)(μ-κ(2)N(2)N(3)-L(1))(μ-CO)(3)(CO)(7)] (1), which contains an intact phthalazine ligand in an axial position bridging an Ru-Ru edge through both N atoms, is initially formed but it reacts with more phthalazine to give [Ru(3)(κN(2)-L(1))(μ-κ(2)N(2)N(3)-L(1))(μ-CO)(3)(CO)(6)] (2), in which a π-π stacking interaction between the aromatic rings of both ligands determines their position in cluster axial sites on the same face of the Ru(3) triangle. With quinazoline (HL(2)), the cyclometalated hydrido decacarbonyl derivative [Ru(3)(μ-H)(μ-κ(2)N(3)C(4)-L(2))(CO)(10)] (3) is initially produced but it partially decarbonylates under the reaction conditions to give [Ru(6)(μ-H)(2)(μ-κ(2)N(3)C(4)-L(2))(μ(3)-κ(3)-N(1)N(3)C(4)-L(2))(CO)(19)] (4), which results from the displacement of a CO ligand of 3 by the uncoordinated N(1) atom of another molecule of 3. With 4,7-phenanthroline (H(2)L(3)), the stepwise formation of the cyclometalated derivatives [Ru(3)(μ-H)(μ-κ(2)N(4)C(3)-HL(3))(CO)(10)] (5) and two isomers of [Ru(6)(μ-H)(2)(μ(4)-κ(4)N(4)C(3)N(7)C(8)-L(3))(CO)(20)] (6a, 6b) takes place. In compounds 6a and 6b, two Ru(3)(μ-H)(CO)(10) trinuclear units are symmetrically (C(2) in 6a or C(S) in 6b) bridged by a doubly-cyclometalated 4,7-phenanthroline ligand. With 2,3'-bipyridine (HL(4)), two products have been isolated, [Ru(3)(μ-H)(μ-κ(2)N(3')C(4')-L(4))(CO)(10)] (7) and [Ru(3)(μ-H)(μ-κ(3)N(2)N(3')C(2')-L(4))(CO)(9)] (8). While compound 7 contains an N(3')C(4')-cyclometalated 2,3'-bipyridine, in compound 8 an N(3')C(2')-cyclometalation is accompanied by the coordination of the N(2) atom of the remaining pyridine fragment. The structures of compounds 2, 3, 4, 6a and 8 have been determined by X-ray diffraction crystallography.

  17. Synthesis of [3 alpha-3H]7-dehydrocholesterol via stable tritiated 4-phenyl-1,2,4-triazoline-3,5-dione derivative.

    PubMed

    Batta, A K; Salen, G; Tint, G S; Honda, A; Shefer, S

    1997-11-01

    Synthesis of [3 alpha-3H]7-dehydrocholesterol is described via protection of the 5,7-diene system in 7-dehydrocholesterol as the Diels-Alder adduct with 4-phenyl-1,2,4-triazoline-3,5-dione followed by oxidation of the hydroxyl group to give the 3-oxo adduct. Reduction of the keto adduct with [3H]sodium borohydride produced the adduct of [3 alpha-3H]7-dehydrocholesterol from which the radiolabeled sterol was obtained via treatment with lithium aluminum hydride. The advantage of the method is that highly labeled [3 alpha-3H]7-dehydrocholesterol can be prepared. Further, unlike 7-dehydrocholesterol, its adduct with 4-phenyl-1,2,4-triazoline-3,5-dione is stable and can be stored. This allows the preparation of small batches of [3 alpha-3H]7-dehydrocholesterol for immediate use in biological experiments, and losses due to decomposition of excess radiolabeled 7-dehydrocholesterol are minimized.

  18. Thermally stable compositions including 2,4,8,10-tetranitro-5H-pyrido[3',2':4,5][1,2,3]triazolo[1,2-a]benzotriazo- l-6-ium, inner salt

    DOEpatents

    Hiskey, Michael A.; Huynh, My Hang

    2010-01-26

    An explosive formulation including 2,4,8,10-tetranitro-5H-pyrido[3',2':4,5][1,2,3]triazolo[1,2-a]benzotriazo- l-6-ium, inner salt and a high temperature binder is disclosed together with a process of preparing 2,4,8,10-tetranitro-5H-pyrido[3',2':4,5][1,2,3]triazolo[1,2-a]benzotriazo- l-6-ium, inner salt.

  19. 2,2,6,6-Tetra-bromo-3,4,4,5-tetra-meth-oxy-cyclo-hexa-none.

    PubMed

    Faizi, Md Serajul Haque; Mashrai, Ashraf; Shahid, M

    2014-07-01

    In the title compound, C10H14Br4O5, synthesized from the meth-oxy Schiff base N-(pyridin-2-ylmeth-yl)meth-oxy-aniline and mol-ecular bromine, the cyclo-hexa-none ring has a chair conformation with one of the four meth-oxy groups equatorially orientated with respect to the carbonyl group and the others axially orientated. The C-Br bond lengthsvary from 1.942 (4) to1.964 (4) Å. In the crystal, weak C-H⋯Ocarbon-yl hydrogen-bonding inter-actions generate chains extending along the b-axis direction. Also present in the structure are two short inter-molecular Br⋯Ometh-oxy inter-actions [3.020 (3) and 3.073 (4) Å].

  20. Cytotoxicity and bioactivation mechanism of benzyl 2-chloro-1,1,2-trifluoroethyl sulfide and benzyl 1,2,3,4,4-pentachlorobuta-1,3-dienyl sulfide

    SciTech Connect

    Veltman, J.C.; Dekant, W.; Guengerich, F.P.; Anders, M.W.

    1988-01-01

    The metabolism and cytotoxicity of benzyl 1,2,3,4,4-pentachlorobuta-1,3-dienyl sulfide (1) and benzyl 2-chloro-1,1,2-trifluoroethyl sulfide (2) were studied as an alternative test of the hypothesis that the toxicity of the cysteine S-conjugates S-(pentachlorobutadienyl)-L-cysteine and S-(2-chloro-1,1,2-trifluoroethyl)-L-cysteine is associated with their metabolism to unstable thiols; the expectation was that the benzyl sulfides 1 and 2 would undergo cytochrome P-450 dependent benzylic hydroxylation and that the intermediate hemimercaptals would eliminate unstable, cytotoxic thiols. This expectation was realized: 1 and 2 were cytotoxic in isolated rat hepatocytes. The cytotoxicity of 1 was greater in hepatocytes from phenobarbital-treated rats compared with control rats and in male then in female rats and was inhibited by carbon monoxide and 2-(N,N-diethylamino)ethyl 2,2-diphenylvalerate HCl (SKF 525-A). Benzyl sulfides 1 and 2 were metabolized to benzaldehyde by rat hepatic microsomal fractions and by a purified, reconstituted cytochrome P-450/sub PB-B/ system. Benzaldehyde was not cytotoxic. These results provide support for the hypothesis that benzyl sulfides 1 and 2 and the corresponding cysteine S-conjugates yield unstable thiols, which may give rise to acylating agents or to stable, but toxic, terminal products that are responsible for the cytotoxic effects of benzyl sulfides and cysteine S-conjugates.

  1. Growth, Thermal and Spectral Properties of Er3+-Doped and Er3+/Yb3+-Codoped Li3Ba2La3(WO4)8 Crystals

    PubMed Central

    Xiao, Bin; Lin, Zhoubin; Zhang, Lizhen; Huang, Yisheng; Wang, Guofu

    2012-01-01

    This paper reports the growth and spectral properties of Er3+-doped and Er3+/Yb3+-codoped Li3Ba2La3(WO4)8 crystals. The Er3+: Li3Ba2La3(WO4)8 crystal with dimensions of 56 mm×28 mm×9 mm and Er3+/Yb3+: Li3Ba2La3(WO4)8 crystal with dimensions of 52 mm×24 mm×8 mm were obtained by the top-seeded solution growth (TSSG) method. Thermal expansion coefficients and thermal conductivity of both crystals were measured. The spectroscopic characterizations of both crystals were investigated. The spectroscopic analysis reveals that the Er3+/Yb3+: Li3Ba2La3(WO4)8 crystal has much better optical properties than the Er3+: Li3Ba2La3(WO4)8 crystal, thus it may become a potential candidate for solid-state laser gain medium material. PMID:22808214

  2. Microbial hydroxylation of o-bromophenylacetic acid: synthesis of 4-substituted-2,3-dihydrobenzofurans.

    PubMed

    Deshpande, Prashant P; Nanduri, Venkata B; Pullockaran, Annie; Christie, Hamish; Mueller, Richard H; Patel, Ramesh N

    2008-08-01

    Microbial hydroxylation of o-bromophenylacetic acid provided 2-bromo-5-hydroxyphenylacetic acid. This enabled a route to the key intermediate 4-bromo-2,3-dihydrobenzofuran for synthesizing a melatonin receptor agonist and sodium hydrogen exchange compounds. Pd-mediated coupling reactions of 4-bromo-2,3-dihydrobenzofuran provided easy access to the 4-substituted-2,3-dihydrobenzofurans.

  3. Crystal structure of 4,5-bis-(3,4,5-tri-meth-oxy-phen-yl)-2H-1,2,3-triazole methanol monosolvate.

    PubMed

    Madadi, Nikhil Reddy; Penthala, Narsimha Reddy; Bommagani, Shobanbabu; Parkin, Sean; Crooks, Peter A

    2014-10-01

    The title compound, C20H23N3O6·CH3OH, was synthesized by [3 + 2] cyclo-addition of (Z)-2,3-bis-(3,4,5-tri-meth-oxy-phen-yl)acrylo-nitrile with sodium azide and ammonium chloride in DMF/water. The central nitro-gen of the triazole ring is protonated. The dihedral angles between the triazole ring and the 3,4,5-tri-meth-oxy-phenyl ring planes are 34.31 (4) and 45.03 (5)°, while that between the 3,4,5-tri-meth-oxy-phenyl rings is 51.87 (5)°. In the crystal, the mol-ecules, along with two methanol solvent mol-ecules are linked into an R (4) 4(10) centrosymmetric dimer by N-H⋯O and O-H⋯N hydrogen bonds.

  4. Nitro group photoreduction of 4-(2-nitrophenyl)- and 4-(3-nitrophenyl)-1,4-dihydropyridines

    NASA Astrophysics Data System (ADS)

    Görner, Helmut

    2010-08-01

    The photoprocesses of nifedipine, a 4-(2-nitrophenyl)-1,4-dihydropyridine, and nimodipine and nitrendipine, two 3-nitrophenyl Hantzsch-type analogues, were studied by steady-state and time-resolved methods. The intramolecular photoreduction of nifedipine into its nitrosophenyl product takes place within a few ns. The quantum yield of conversion is Φred = 0.3 and does not depend significantly on the oxygen concentration and solvent properties. Formation of the fully reduced 4-(2-aminophenyl)-1,4-dihydropyridine as minor product is indicated by fluorescence spectroscopy. The photoreduction of nimodipine and nitrendipine is inefficient, Φred = 0.002 in acetonitrile, but markedly enhanced in the presence of donors such as triethylamine (TEA) and 2-propanol, e.g. for TEA Φred is up to 0.03. The triplet states of nimodipine and nitrendipine were characterized. They react intermolecularly with TEA and 2-propanol, forming radicals as intermediates and eventually several reduction products.

  5. N'-[1-(2,4-Dioxo-3,4-dihydro-2H-1-benzopyran-3-yl-idene)eth-yl]thiophene-2-carbo-hydrazide.

    PubMed

    Helliwell, Madeleine; Nasiopoulou, Despina A; Harris, Philip A; Kotali, Antigoni; Joule, John A

    2011-04-01

    The title compound, C(16)H(12)N(2)O(4)S, was obtained by the condensation of 3-acetyl-4-hy-droxy-coumarin with thien-2-ylcarbonyl hydrazide. The pyran ring adopts a 2,4-dione tautomeric form. The benzopyran ring system is almost coplanar with the thio-phene ring [dihedral angle 0.9 (2)°]. The exocyclic C=C double bond has an E geometry. The mol-ecular conformation is stabilized by an intra-molecular N-H⋯O hydrogen bond. In the crystal, inter-molecular N-H⋯O hydrogen bonds link the mol-ecules into chains along the a axis.

  6. Synthesis and pharmacological investigation of 2-(4-dimethylaminophenyl)-3,5-disubstituted thiazolidin-4-ones as anticonvulsants.

    PubMed

    Senthilraja, Manavalan; Alagarsamy, Veerachamy

    2012-10-01

    A new series of 2-(4-dimethylaminophenyl)-3-substituted thiazolidin-4-one-5-yl-acetyl acetamides/benzamides were synthesized by the nucleophilic substitution of 3-substituted-2-(4-dimethylaminophenyl)-thiazolidin-4-one-5-yl-acetylchloride with acetamide and benzamide. The starting material 3-substituted-2-(4-dimethylaminophenyl)-thiazolidin-4-one-5-yl-acetylchloride was synthesized from 3-substituted-2-(4-dimethylaminophenyl)-thiazolidin-4-one-5-yl-acetic acid, which in turn was prepared by one-pot reaction of amino component, p-dimethylamino benzaldehyde and mercapto succinic acid. The title compounds were investigated for their anticonvulsant activities; among the test compounds, compound 2-(4-dimethylaminophenyl)-3-phenylamino-thiazolidine-4-one-5-yl-acetylbenzamide (14) emerged as the most active compound of the series and as moderately more potent than the reference standard diazepam.

  7. Ternary chalcogenides Cs2Zn3Se4 and Cs2Zn3Te4 : Potential p -type transparent conducting materials

    DOE PAGES

    Shi, Hongliang; Saparov, Bayrammurad; Singh, David J.; ...

    2014-11-11

    Here we report prediction of two new ternary chalcogenides that can potentially be used as p-type transparent conductors along with experimental synthesis and initial characterization of these previously unknown compounds, Cs2Zn3Ch4 (Ch = Se, Te). In particular, the structures are predicted based on density functional calculations and confirmed by experiments. Phase diagrams, electronic structure, optical properties, and defect properties of Cs2Zn3Se4 and Cs2Zn3Te4 are calculated to assess the viability of these materials as p-type TCMs. Cs2Zn3Se4 and Cs2Zn3Te4, which are stable under ambient air, display large optical band gaps (calculated to be 3.61 and 2.83 eV, respectively) and have smallmore » hole effective masses (0.5-0.77 me) that compare favorably with other proposed p-type TCMs. Defect calculations show that undoped Cs2Zn3Se4 and Cs2Zn3Te4 are p-type materials. However, the free hole concentration may be limited by low-energy native donor defects, e.g., Zn interstitials. Lastly, non-equilibrium growth techniques should be useful for suppressing the formation of native donor defects, thereby increasing the hole concentration.« less

  8. Co-precipitation synthesis of Y2O2SO4:Eu3+ nanophosphor and comparison of photoluminescence properties with Y2O3:Eu3+ and Y2O2S:Eu3+ nanophosphors

    NASA Astrophysics Data System (ADS)

    Lian, Jingbao; Qin, Hua; Liang, Ping; Liu, Feng

    2015-10-01

    Eu3+ ions activated yttrium oxysulfate (Y2O2SO4:Eu3+) nanophosphor has been successfully synthesized by a co-precipitation method from commercially available Y(NO3)3·6H2O, Eu(NO3)3·6H2O, (NH4)2SO4 and NH3·H2O as the starting materials. Detailed characterizations of the synthetic products were obtained by differential thermal analysis, thermogravimetry and derivative thermogravimetry (DTA-TG-DTG), Fourier transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), transmission electron microscopy (TEM), and photoluminescence (PL) spectroscopy. The results revealed that the precursor was composed of amorphous yttrium hydroxide sulfate when (NH4)2SO4 was introduced in the reaction system. Moreover, the precursor could be converted into pure Y2O2SO4 phase by calcining at 800 °C for 2 h in air and pure Y2O2S phase could be obtained by calcining Y2O2SO4 at 800 °C for 1 h in hydrogen atmosphere. The as-synthesized Y2O2SO4 phosphor particles are quasi-spherical in shape, slight aggregation and about 20-30 nm in size. PL spectra of the Y2O2SO4:Eu3+ nanophosphor under 270 nm ultraviolet (UV) light excitation show a red emission at 620 nm as the most prominent peak, which attributes to the 5D0→7F2 transition of Eu3+ ions. The quenching concentration of Eu3+ ions was 5 mol%, and its corresponding fluorescence lifetime was 1.49 ms according to the linear fitting result. Furthermore, the Y2O3 nanophosphor was synthesized by similar reaction and comparison of PL properties among three kinds of Eu3+ activated nanophosphors was also systematically discussed.

  9. Crystal structure of ethyl (E)-4-(4-chlorophen-yl)-4-meth-oxy-2-oxobut-3-enoate.

    PubMed

    Flores, Darlene Correia; Vicenti, Juliano Rosa de Menezes; Pereira, Bruna Ávila; da Silva, Gabriele Marques Dias; Zambiazi, Priscilla Jussiane

    2014-09-01

    In the title compound, C13H13ClO4, the dihedral angle between the chloro-benezene ring and the least-squares plane through the 4-meth-oxy-2-oxobut-3-enoate ethyl ester residue (r.m.s. deviation = 0.0975 Å) is 54.10 (5)°. In the crystal, mol-ecules are connected by meth-oxy-ketone and benzene-carboxyl-ate carbonyl C-H⋯O inter-actions, generating a supra-molecular layer in the ac plane.

  10. Interfaces exchange bias and magnetic properties of ordered CoFe2O4/Co3O4 nanocomposites

    NASA Astrophysics Data System (ADS)

    Zhang, B. B.; Xu, J. C.; Wang, P. F.; Han, Y. B.; Hong, B.; Jin, H. X.; Jin, D. F.; Peng, X. L.; Li, J.; Yang, Y. T.; Gong, J.; Ge, H. L.; Wang, X. Q.

    2015-11-01

    Cobalt ferrites (CoFe2O4) nanoparticles were implanted into the ordered mesoporous cobaltosic oxide (Co3O4) nanowires to synthesize magnetic CoFe2O4/Co3O4 nanocomposites. X-ray diffraction (XRD), N2 physical absorption-desorption, transmission electron microscope (TEM) and energy disperse spectroscopy (EDS) were used to characterize the microstructure of mesoporous Co3O4 and CoFe2O4/Co3O4 nanocomposites. The percent of pore-volume of mesoporous Co3O4 nanowires was calculated to be about 41.99% and CoFe2O4 nanoparticles were revealed to exist in the mesopores of Co3O4. The magnetic behavior of both samples were investigated with superconducting quantum interference device (SQUID). Magnetization increased with the doping CoFe2O4 and decreasing temperature, while coercivity hardly changed. The exchange bias effect was obviously observed at 100 K and enhanced with the doping CoFe2O4. CoFe2O4 nanoparticles reinforced the interfaces magnetic interaction between antiferromagnetic Co3O4 and ferrimagnetic CoFe2O4.

  11. Synthesis of 3-amino-6-methyl-5-ethoxycarbonyl-4,7-dihydrothieno(2,3-b)pyridine derivatives

    SciTech Connect

    Krauze, A.A.; Liepin'sh, E.E.; Pelcher, Yu.E.; Dubur, G.Ya.

    1987-07-01

    The alkylation of piperidinium salts of substituted 1,4-dihydropyridine-2-thiols with chloroacetonitrile or iodoacetamide gave 2-cyanomethylthio- and 2-carbamoylmethylthio-substituted 6-methyl-4-acryl(pyridyl)-5-ethoxycarbonyl-3-cyano-1,4-dihydropyridines, which undergo intramolecular cyclization in basic media to give 3-amino-6-methyl-4-aryl(pyridyl)-5-ethoxycarbonyl-2-cyano(carbamoyl)-4,7-dihydrothieno(2,3-b)pyridines.

  12. 42 CFR 84.100 - Man tests 1, 2, 3, and 4; requirements.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ...-Contained Breathing Apparatus § 84.100 Man tests 1, 2, 3, and 4; requirements. Man tests 1, 2, 3, and 4, set... of work and physical orientation; and (d) Provide information on the operating and...

  13. 42 CFR 84.100 - Man tests 1, 2, 3, and 4; requirements.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ...-Contained Breathing Apparatus § 84.100 Man tests 1, 2, 3, and 4; requirements. Man tests 1, 2, 3, and 4, set... of work and physical orientation; and (d) Provide information on the operating and...

  14. 42 CFR 84.100 - Man tests 1, 2, 3, and 4; requirements.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ...-Contained Breathing Apparatus § 84.100 Man tests 1, 2, 3, and 4; requirements. Man tests 1, 2, 3, and 4, set... of work and physical orientation; and (d) Provide information on the operating and...

  15. 42 CFR 84.100 - Man tests 1, 2, 3, and 4; requirements.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ...-Contained Breathing Apparatus § 84.100 Man tests 1, 2, 3, and 4; requirements. Man tests 1, 2, 3, and 4, set... of work and physical orientation; and (d) Provide information on the operating and...

  16. 42 CFR 84.100 - Man tests 1, 2, 3, and 4; requirements.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ...-Contained Breathing Apparatus § 84.100 Man tests 1, 2, 3, and 4; requirements. Man tests 1, 2, 3, and 4, set... of work and physical orientation; and (d) Provide information on the operating and...

  17. [Dimethyl 3-benzyl-2-(4-methyl-2,5-dioxoimidazolidin-1-yl)butanedioate].

    PubMed

    Rolland, M; Jenhi, A; Lavergne, J P; Martinez, J; Hasnaoui, A

    2001-01-01

    There are two symmetry-independent formula units of the title compound, dimethyl 3-benzyl-2-(4-methyl-2,5-dioxoimidazolidin-1-yl)butanedioate, C17)H20N2O6, per cell. The two symmetry-independent molecules differ in their configuration and are diastereomers. This structural study confirms a new side reaction during the synthesis of seven-membered cyclopeptides. The stereochemistry of both diastereomers has been established.

  18. Synthesis and characterization of Li 3V (2 - 2 x/3)Mg x(PO 4) 3/C cathode material for lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Huang, J. S.; Yang, L.; Liu, K. Y.; Tang, Y. F.

    Li 3V (2 - 2 x/3)Mg x(PO 4) 3/C (x = 0, 0.15, 0.30, 0.45) composites have been synthesized by the sol-gel assisted solid state method, using adipic acid C 6H 10O 4 (hexanedioic acid) as carbon source. The particle size of the composites is ∼1 μm. During the pyrolysis process, Li 3V (2 - 2 x/3)Mg x(PO 4) 3/C network structure is formed. The effect of Mg 2+ doped on the electrochemical properties of Li 3V 2(PO 4) 3/C positive materials has been studied. Li 3V 1.8Mg 0.30(PO 4) 3/C as the cathode materials of Li-ion batteries, the retention rate of discharge capacity is 91.4% (1 C) after 100 cycles. Compared with Li 3V 2(PO 4) 3/C, Li 3V (2 - 2 x/3)Mg x(PO 4) 3/C composites have shown enhanced capacity and retention rate capability. The long-term cycles and ex situ XRD tests disclose that Li 3V 1.8Mg 0.30(PO 4) 3 exhibits higher structural stability than the undoped system.

  19. Vibration and DFT analysis of 2-methyl-3-nitrophenyl isocyanate and 4-methyl-2-nitrophenyl isocyanate.

    PubMed

    Tonannavar, J; Prasannakumar, Sushanti; Savanur, J; Yenagi, Jayashree

    2012-09-01

    Vibrational spectra of 2-methyl-3-nitrophenyl isocyanate and 4-methyl-2-nitrophenyl isocyanate, in the spectral region 4000-100 cm(-1), have been measured and assigned. Conformational and harmonic frequency analyses have been performed at B3LYP/6-311G(∗) level of calculations. The two stable conformers, cis and trans, have been computed for each of the molecules. It has been determined that the trans conformer has lower energy than the cis by 3.954 kJ/mol for 2-methyl-3-nitrophenyl isocyanate; whereas the cis conformer has lower energy than the trans by 10.230 kJ/mol for 4-methyl-2-nitrophenyl isocyanate. The vibration structure of 2-methyl-3-nitrophenyl isocyanate conforms to the combined behavior of its both conformers from which the deviation is shown by the structure of 4-methyl-2-nitrophenyl isocyanate which follows only the trans conformer. The occurrence of symmetric mode of the methyl group at higher frequency near 2944-20 cm(-1) is attributed to the phenyl ring strain caused by the substituents. As for the other stretching and bending modes, mutually exclusive pattern appears to work for the molecules: The nitro group's non-coplanarity with the phenyl ring is more evident in 4-methyl-2-nitrophenyl isocyanate where the asymmetric mode was assigned to the band at 1569cm(-1), whereas the symmetric mode at lower frequency 1339cm(-1). Occasional doublet appearance of the strong asymmetric absorption near 2282cm(-1) due to isocyanate moiety has been observed in the present study and is assumed to arise from the torsional vibration motion of the moiety rendered by the small energy gap between the conformers of 2-methyl-3-nitrophenyl isocyanate.

  20. Stabilizing Superacid Anions: The New [H(S4 O13 )2 ](3-) Anion in the Crystal Structure of Li3 [H(S4 O13 )2 ].

    PubMed

    Schindler, Lisa Verena; Becker, Anna; Wickleder, Mathias Siegfried

    2016-12-05

    The unique hydrogenium-bis-tetrasulfate anion [H(S4 O13 )2 ](3-) in the crystal structure of Li3 [H(S4 O13 )2 ] (monoclinic, P21 /n (No. 14), Z=2, a=552.46(4) pm, b=939.70(6) pm, c=1876.6(1) pm, β=97.492(3)°, V=965.9(1)⋅10(6)  pm(3) ) is the longest protonated polysulfate chain ever observed. Very strong symmetrical hydrogen bonds are a bold feature of the crystal structure. The protonation of a very weak base such as [S4 O13 ](2-) and accordingly the stabilization of the first base of the superacid H2 S4 O13 is a significant success towards the still elusive polysulfuric acids.

  1. Improved photoelectrochemical performance of Z-scheme g-C3N4/Bi2O3/BiPO4 heterostructure and degradation property

    NASA Astrophysics Data System (ADS)

    Li, Junqi; Yuan, Huan; Zhu, Zhenfeng

    2016-11-01

    In g-C3N4/Bi2O3/BiPO4, the p-n junction between p-type Bi2O3 and n-type BiPO4 was encapsulated by g-C3N4 and a direct Z-scheme was built between g-C3N4 and Bi2O3. The optical, morphological and photoelectrochemical (PEC) properties of BiPO4, g-C3N4/BiPO4, Bi2O3/BiPO4 and g-C3N4/Bi2O3/BiPO4 hierarchical Z-scheme system were studied. More than 90% photodegradation of methyl orange (MO) with the exposure of simulated solar light was achieved within 160 min with the g-C3N4/Bi2O3/BiPO4, which displayed remarkably promoted photocatalytic activities than other samples. The electrochemical impedance spectra and photocurrent results also proved that efficient charge separation and better electron transport properties were achieved by g-C3N4/Bi2O3/BiPO4. In general, the addition of g-C3N4 can guide the residual electrons on p-type Bi2O3 to recombine with photoholes of g-C3N4 and make sure the left carries exhibit stronger oxidation and reduction ability to boost the production of active groups.

  2. Reversal modes and magnetostatic interactions in Fe3O4/ZrO2/Fe3O4 multilayer nanotubes.

    PubMed

    Pitzschel, Kristina; Bachmann, Julien; Montero-Moreno, Josep M; Escrig, Juan; Görlitz, Detlef; Nielsch, Kornelius

    2012-12-14

    Reversal modes and magnetostatic interactions of multilayered Fe(3)O(4)/ZrO(2)/Fe(3)O(4) nanotubes consisting of a ferromagnetic internal tube, an intermediate non-magnetic spacer and an external magnetic shell are investigated as a function of their geometric parameters and compared with those produced inside the pores of anodic alumina membranes by atomic layer deposition. Based on a continuum approach we obtained analytical expressions that underline the first experimental results and support their interpretation that the system of multilayer tubes behaves as the reversal of two isolated systems. It is observed that the magnetostatic interaction between both phases depends on the magnetic configurations in each phase and also on the geometrical parameters considered. These structures have potential applications in novel spintronics devices, ultra-small magnetic media and other nano-devices.

  3. Synthesis and anticonvulsant activity of 6-alkoxy-[1,2,4]triazolo[3,4-a]phthalazines.

    PubMed

    Zhang, Lei; Guan, Li-Ping; Sun, Xian-Yu; Wei, Cheng-Xi; Chai, Kyu-Yun; Quan, Zhe-Shan

    2009-03-01

    A new series of 6-alkoxy-[1,2,4]triazolo[3,4-a]phthalazines (3a-3v) were synthesized and their anticonvulsant activity and neurotoxicity were evaluated by the maximal electroshock test and the rotarod test respectively. Significant anticonvulsant activity was displayed by a number of compounds. The most promising compounds 6-(4-chlorobenzyloxy)-[1,2,4]triazolo[3,4-a]phthalazine (3f) and 6-heptyloxy-[1,2,4]triazolo[3,4-a]phthalazine (3s) showed a median effective dose of 7.1 and 11.0 mg/kg, and had protective index value of 5.2 and 8.0 respectively. The two compounds were further found to have potent activity against seizures induced by pentylenetetrazole, isoniazid, thiosemicarbazide, 3-mercaptopropionic acid but not seizures induced by strychnine, indicating that the two compounds might function by enhancing gamma-aminobutyric acid neurotransmission.

  4. Synthesis and characterization of Mn2+ doped CdOZn3(PO4)2 nanocomposites

    NASA Astrophysics Data System (ADS)

    Naga Bhaskararao, Y.; Satyavathi, K.; Subba Rao, M.; Cole, Sandhya

    2017-02-01

    Undoped and Mn2+ doped CdOZn3(PO4)2 nanocomposites are fruitfully synthesized by chemical precipitation process at room temperature. The morphology, structure and spectroscopic properties of the prepared samples are characterized by X-ray diffraction (XRD), optical absorption, Scanning electron microscope (SEM) with EDS, Fourier transform infrared (FT-IR) spectroscopy, Photolumiscence (PL) and Electron Paramagnetic Resonance (EPR). XRD data confirms the cubic phase of CdO and monoclinic phase of Zn3(PO4)2. Strain and dislocation density are also calculated from XRD studies. Optical absorption spectrum of Mn2+ doped CdOZn3(PO4)2 nanocomposite shows different spin-forbidden DMSO-d6 bands which are the characteristics of octahedral site symmetry related to Mn2+. The crystal field parameter Dq and inter electronic repulsion parameters (B and C) are deliberate using optical absorption data. Surface morphology of sample is firm by Using Scanning electron microscopy (SEM) and the distribution of Zn, Cd, phosphate and oxygen species in the prepared sample is identified by EDS. PL studies recognize the white light emission. The 'g' value of the nanocomposite material synthesized is lesser than (negative shift) the free electron value (2.0023), which gives ionic nature to the bonding and confirms the presence of Mn2+ in distorted octahedral site symmetry.

  5. Visible light photoredox catalysis: synthesis of indazolo[2,3-a]quinolines from 2-(2-nitrophenyl)-1,2,3,4-tetrahydroquinolines.

    PubMed

    Lin, Wen-Chung; Yang, Ding-Yah

    2013-09-20

    The synthesis of indazolo[2,3-a]quinoline derivatives in moderate to good yields from 2-(2-nitrophenyl)-1,2,3,4-tetrahydroquinolines via visible light photoredox catalysis is reported. The reaction involves a novel ruthenium-catalyzed intramolecular formation of the N-N bond of the indazole ring.

  6. Mutagenicity in Salmonella and sister chromatid exchange in mice for 1,4-, and 1,3-, 2,4-, and 3,4-dimethylphenanthrenes

    SciTech Connect

    Sinsheimer, J.E.; Giri, A.K.; Hooberman, B.H.; Jung, K.Y.; Gopalaswamy, R.; Koreeda, M. )

    1991-01-01

    The mutagenicity in Salmonella and in vivo sister chromatid exchange in the bone-marrow cells of mice was determined for 1,4-, 1,3-, 2,4-, and 3,4-dimethylphenanthrene (DMPh) with the objective to study the relative importance of substitution at the 1 and 4 positions of this series of methylated phenanthrenes. For both tests, 1,4-DMPh was decidedly more genotoxic than the remaining regioisomers. While the well recognized role of steric crowding in the bay region is a factor in this enhanced genotoxicity, equally important is substitution at the 1 position with its potential to inhibit detoxication through 9,10-diol formation.

  7. 3-(Triphenylphosphoranylidene)pentane-2,4-dione and diethyl 2-(triphenylphosphoranylidene)malonate.

    PubMed

    Castañeda, Fernando; Aliaga, Christian; Bunton, Clifford A; Garland, María Teresa; Baggio, Ricardo

    2005-08-01

    The title ylides, 3-(triphenylphosphoranylidene)pentane-2,4-dione, C23H21O2P, (I), and diethyl 2-(triphenylphosphoranylidene)malonate, C25H25O4P, (II), differ in the conformations adopted by their extended ylide moieties. In (I), one carbonyl O atom is syn and the other is anti with respect to the P atom, the ylide group is nearly planar, with a maximum P-C-(C=O) angle of 18.2 (2)degrees, and the P-C, C-C and C=O bond lengths are consistent with electronic delocalization involving the O atoms. In (II), both carbonyl O atoms are anti and the ester groups are twisted out of the plane of the near trigonal ylide C atom, reducing delocalization, the largest P-C-(C=O) angle being 30.2 (2)degrees.

  8. Crystal structures of [Ln(NO3)32-bpydo)2], where Ln = Ce, Pr or Nd, and bpydo = 4,4'-bi-pyridine N,N'-dioxide: layered coordination networks containing 4(4) grids.

    PubMed

    Stromyer, Michael L; Lilly, Cassandra P; Dillner, Adam J; Knaust, Jacqueline M

    2016-01-01

    Three isostructural coordination networks of Ce, Pr, and Nd nitrate with 4,4'-bi-pyridine N,N'-dioxide (bpydo) are reported, namely poly[[tris-(nitrato-κ(2) O,O')cerium(III)]-bis-(μ2-4,4'-bi-pyridine N,N'-dioxide-κ(2) N:N')], [Ce(NO3)3(C10H8N2O2)2], poly[[tris-(nitrato-κ(2) O,O')praeseodymium(III)]-bis-(μ2-4,4'-bi-pyridine N,N'-dioxide-κ(2) N:N')], [Pr(NO3)3(C10H8N2O2)2], and poly[[tris(nitrato-κ(2) O,O')neodymium(III)]-bis-(μ2-4,4'-bi-pyridine N,N'-dioxide-κ(2) N:N'], [Nd(NO3)3(C10H8N2O2)2]. All three compounds are isostructural to the previously reported La analogue. The asymmetric unit of [Ln(NO3)32-bpydo)2] contains one lanthanide cation, two bpydo ligands, and three nitrate anions. Both bpydo ligands act as end-to-end μ2-bridges and display nearly ideal cis and gauche conformations, respectively. The bpydo ligands link the ten-coordinate Ln (III) cations, forming inter-digitating 4(4) grid-like layers extending parallel to (-101), where inter-digitation of layers is promoted by C-H⋯O inter-actions between nitrate anions and bpydo ligands. The inter-digitated layers are linked to sets of neighboring layers via further C-H⋯O and π-π inter-actions.

  9. Formation of a highly stable complex between BN 50730 [tetrahydro-4,7,8,10 methyl-1(chloro-2 phenyl)-6 (methoxy-4 phenyl-carbamoyl)-9 pyrido [4',3'-4,5] thieno [3,2-f] triazolo-1,2,4 [4,3-a] diazepine-1,4] and the platelet-activating factor receptor in rabbit platelet membranes.

    PubMed

    Silva, C L; Cruz, H N; Violante, F A; Cordeiro, R S; Martins, M A; Noël, F

    1996-01-26

    BN 50730 [tetrahydro-4,7,8,10 methyl-1(chloro-2 phenyl)-6 (methoxy-4 phenyl-carbamoyl)-9 pyrido [4',3'-4,5] thieno [3,2-f] triazolo-1,2,4 [4,3-alpha] diazepine-1,4], a novel platelet-activating factor (PAF) receptor antagonist with a hetrazepine structure, decreased the maximal number of binding sites (Bmax) of [3H]PAF in rabbit platelet membranes without altering its dissociation constant. Platelet aggregation induced by 1 microM PAF was prevented by preincubation with 1 microM BN 50730. The washing of the platelets preincubated with BN 50730 failed to revert its inhibitory effects. We conclude that BN 50730 acts as a non-competitive antagonist of the PAF receptor, due to the formation of a highly stable drug-receptor complex.

  10. Structural and theoretical study on the 1:2 addition complex of 1,2,4,5-bis{8‧,11‧-dithia[4.3.3]propella(3‧,4‧)}benzene with I2

    NASA Astrophysics Data System (ADS)

    Szlachcic, Paweł; Seidler, Tomasz; Stadnicka, Katarzyna

    2013-02-01

    The crystal structure of the title compound, C22H26S4·2I2, contains two centrosymmetric molecules of 1,2,4,5-bis{8',11'-dithia[4.3.3]propella(3',4')}benzene, and four I2 molecules in the unit cell of space group P21/c. The cyclohexene rings adopt boat conformation, whereas tetrahydrothiophene rings have envelope conformation. The iodine molecules are linked to one type of the sulphur atoms of the propellane molecule by a charge-transfer bond, with S⋯I distance of 2.7844(12) and I-I = 2.8153(5) Å. The second type of symmetrically independent sulphur atoms are engaged in a weak interaction of C-H⋯S type with the H⋯S distance of 3.09(1) Å. The geometry optimisation of the crystal structure at the B3LYP level with MIDI! basis set gave good agreement with the experimental data (S⋯I distance of 2.754 and I-I = 2.923 Å). NBO analysis for the complex showed that the S⋯I interaction is due to charge transfer from the lone pair on the sulphur to the vacant σ* orbital of the I2 acceptor.

  11. Bis(5-amino-3-carb­oxy-1H-1,2,4-triazol-4-ium) dihydrogenphosphate nitrate 5-amino-1H-1,2,4-triazol-4-ium-3-carboxyl­ate

    PubMed Central

    Berrah, Fadila; Bouchene, Rafika; Bouacida, Sofiane; Daran, Jean-Claude

    2012-01-01

    In the title compound, 2C3H5N4O2 +·H2PO4 −·NO3 −·C3H4N4O2, three independent 5-amino-1H-1,2,4-triazol-3-carb­oxy­lic acid moieties are observed. Two are in the form of cations, while the third is in the zwitterionic form. The triazole rings in the two cations are almost coplanar, making an angle of 4.11 (7)°. Layers parallel to the (20-1) plane, resulting from hydrogen bonding of the organic mol­ecules and the nitrate anions, are linked via H2PO4 − infinite zigzag chains running parallel to the c axis. The crystal studied was an inversion twin, with refined components of 0.33 (7) and 0.67 (7). PMID:22590233

  12. Crystal structure and magnetic properties of Li,Cr-containing molybdates Li 3Cr(MoO 4) 3, LiCr(MoO 4) 2 and Li 1.8Cr 1.2(MoO 4) 3

    NASA Astrophysics Data System (ADS)

    Sarapulova, A.; Mikhailova, D.; Senyshyn, A.; Ehrenberg, H.

    2009-12-01

    Single crystals of LiCr(MoO 4) 2, Li 3Cr(MoO 4) 3 and Li 1.8Cr 1.2(MoO 4) 3 were grown by a flux method during the phase study of the Li 2MoO 4-Cr 2(MoO 4) 3 system at 1023 K. LiCr(MoO 4) 2 and Li 3Cr(MoO 4) 3 single phases were synthesized by solid-state reactions. Li 3Cr(MoO 4) 3 adopts the same structure type as Li 3In(MoO 4) 3 despite the difference in ionic radii of Cr 3+ and In 3+ for octahedral coordination. Li 3Cr(MoO 4) 3 is paramagnetic down to 7 K and shows a weak ferromagnetic component below this temperature. LiCr(MoO 4) 2 is isostructural with LiAl(MoO 4) 2 and orders antiferromagnetically below 20 K. The magnetic structure of LiCr(MoO 4) 2 was determined from low-temperature neutron diffraction and is based on the propagation vektor k⇒=({1}/{2},{1}/{2},0). The ordered magnetic moments were refined to 2.3(1) μ B per Cr-ion with an easy axis close to the [1 1 1¯] direction. A magnetic moment of 4.37(3) μ B per Cr-ion was calculated from the Curie constant for the paramagnetic region. The crystal structures of the hitherto unknown Li 1.8Cr 1.2(MoO 4) 3 and LiCr(MoO 4) 2 are compared and reveal a high degree of similarity: In both structures MoO 4-tetrahedra are isolated from each other and connected with CrO 6 and LiO 5 via corners. In both modifications there are Cr 2O 10 fragments of edge-sharing CrO 6-octahedra.

  13. 2,4,6-Tris(2,2,2-trinitroethylamino)-1,3,5-triazine: Synthesis, Characterization, and Energetic Properties

    NASA Astrophysics Data System (ADS)

    Li, Shenghua; Zhang, Weiwei; Wang, Yuan; Zhao, Xiuxiu; Zhang, Lubo; Pang, Siping

    2014-05-01

    A simple and straightforward route for the synthesis of 2,4,6-tris(2,2,2-trinitroethylamino)-1,3,5-triazine (TTET) has been developed. The compound was fully characterized by multinuclear (1H, 13C) magnetic resonance and infrared (IR) spectroscopy, elemental analysis, electron ionization-mass spectrometry, and differential scanning calorimetry (DSC). TTET was found to have good physical properties, such as good thermal stability (Td = 186°C), reasonable impact sensitivity (21.5 J), and high density (1.88 g . cm-3). Additionally, the detonation properties of TTET obtained with the empirical Kamlet-Jacobs equations identify it as a competitively energetic compound, which in some cases is superior to 1,3,5-Trinitroperhydro-1,3,5-triazine.

  14. Luminescence properties of long-lasting phosphor SrMg2(PO4)2:Eu2+, Ho3+, Zr4+

    NASA Astrophysics Data System (ADS)

    Tang, Wei; Wang, Mingwen; Lin, Wei; Ye, Yaping; Wu, Xue

    2016-12-01

    Novel long lasting phosphors SrMg2(PO4)2:Eu2+, SrMg2(PO4)2:Eu2+, Zr4+, SrMg2(PO4)2:Eu2+, Ho3+ and SrMg2(PO4)2:Eu2+, Ho3+, Zr4+ were synthesized by conventional solid-state reaction method. The luminescent properties were systematically characterized by X-ray diffraction, photoluminescent excitation and emission spectra, as well as thermoluminescence spectrum and decay curves. The XRD patterns indicated that the samples belonged to monoclinic phase and co-doping Eu2+, Ho3+ and Zr4+ ions had no effect on the basic crystal structure. These phosphors emitting purplish blue light is related to the characteristic emission of Eu2+. The afterglow time of Eu2+ activated SrMg2(PO4)2 can be greatly enhanced by the co-doping of Ho3+, Zr4+. After the 365 nm UV light excitation source switching off, the Sr0.92Mg1.95(PO4)2:Eu2+0.01, Zr4+0.05, Ho3+0.07 phosphorescence can be observed for more than 1013 s in the limit of light perception of dark-adapted human eyes (0.32 mcd/m2). Different kinds of TL peaks at 423, 448 and 473 K have appeared, and traps densities have increased compared with the Eu2+ single doped SrMg2(PO4)2 phosphor. By analyzing the TL curve the depths of traps were calculated to be 0.846, 0.896 and 0.946 eV, respectively, which suggested that the co-doping of Ho3+, Zr4+ improved the electron storage ability of material. Besides, the mechanism was discussed in this report.

  15. Mass spectrometric study of 1,2,4- and 1,3,4-oxadiazoles containing indole substituents

    SciTech Connect

    Ushakova, R.L.; Mikaya, A.I.; Zaikin, V.G.; Kelarev, V.I.; Shveikhgeimer, G.A.

    1986-10-01

    1,2,4- and 1,3,4-Oxadiazoles containing indole substituents decompose upon electron impact due to breakage of bonds in the oxadiazole ring. Skeletal rearrangements may occur in the molecular ions of 2,5-diaryl-1,3,4-oxadiazoles due to migration of the aryl groups.

  16. A Review on Pharmacological Properties of Zingerone (4-(4-Hydroxy-3-methoxyphenyl)-2-butanone).

    PubMed

    Ahmad, Bilal; Rehman, Muneeb U; Amin, Insha; Arif, Ahmad; Rasool, Saiema; Bhat, Showkat Ahmad; Afzal, Insha; Hussain, Ishraq; Bilal, Sheikh; Mir, Manzoor ur Rahman

    2015-01-01

    Humans have been using natural products for medicinal use for ages. Natural products of therapeutic importance are compounds derived from plants, animals, or any microorganism. Ginger is also one of the most commonly used condiments and a natural drug in vogue. It is a traditional medicine, having some active ingredients used for the treatment of numerous diseases. During recent research on ginger, various ingredients like zingerone, shogaol, and paradol have been obtained from it. Zingerone (4-(4-hydroxy-3-methoxyphenyl)-2-butanone) is a nontoxic and inexpensive compound with varied pharmacological activities. It is the least pungent component of Zingiber officinale. Zingerone is absent in fresh ginger but cooking or heating transforms gingerol to zingerone. Zingerone closely related to vanillin from vanilla and eugenol from clove. Zingerone has potent anti-inflammatory, antidiabetic, antilipolytic, antidiarrhoeic, antispasmodic, and so forth properties. Besides, it displays the property of enhancing growth and immune stimulation. It behaves as appetite stimulant, anxiolytic, antithrombotic, radiation protective, and antimicrobial. Also, it inhibits the reactive nitrogen species which are important in causing Alzheimer's disease and many other disorders. This review is written to shed light on the various pharmacological properties of zingerone and its role in alleviating numerous human and animal diseases.

  17. A Review on Pharmacological Properties of Zingerone (4-(4-Hydroxy-3-methoxyphenyl)-2-butanone)

    PubMed Central

    Ahmad, Bilal; Rehman, Muneeb U.; Amin, Insha; Arif, Ahmad; Rasool, Saiema; Bhat, Showkat Ahmad; Afzal, Insha; Hussain, Ishraq; Bilal, Sheikh; Mir, Manzoor ur Rahman

    2015-01-01

    Humans have been using natural products for medicinal use for ages. Natural products of therapeutic importance are compounds derived from plants, animals, or any microorganism. Ginger is also one of the most commonly used condiments and a natural drug in vogue. It is a traditional medicine, having some active ingredients used for the treatment of numerous diseases. During recent research on ginger, various ingredients like zingerone, shogaol, and paradol have been obtained from it. Zingerone (4-(4-hydroxy-3-methoxyphenyl)-2-butanone) is a nontoxic and inexpensive compound with varied pharmacological activities. It is the least pungent component of Zingiber officinale. Zingerone is absent in fresh ginger but cooking or heating transforms gingerol to zingerone. Zingerone closely related to vanillin from vanilla and eugenol from clove. Zingerone has potent anti-inflammatory, antidiabetic, antilipolytic, antidiarrhoeic, antispasmodic, and so forth properties. Besides, it displays the property of enhancing growth and immune stimulation. It behaves as appetite stimulant, anxiolytic, antithrombotic, radiation protective, and antimicrobial. Also, it inhibits the reactive nitrogen species which are important in causing Alzheimer's disease and many other disorders. This review is written to shed light on the various pharmacological properties of zingerone and its role in alleviating numerous human and animal diseases. PMID:26106644

  18. Synthesis of 7-azabicyclo[2.2.1]heptane and 2-oxa-4-azabicyclo[3.3.1]non-3-ene derivatives by base-promoted heterocyclization of alkyl N-(cis(trans)-3,trans(cis)-4-dibromocyclohex-1-yl)carbamates and N-(cis(trans)-3,trans(cis)-4-dibromocyclohex-1-yl)-2,2,2-trifluoroacetamides.

    PubMed

    Gómez-Sanchez, Elena; Soriano, Elena; Marco-Contelles, José

    2007-11-09

    We have studied the base-promoted heterocyclization of alkyl N-(cis(trans)-3,trans(cis)-4-dibromocyclohex-1-yl)carbamates and N-(cis(trans)-3,trans(cis)-4-dibromocyclohex-1-yl)-2,2,2-trifluoroacetamides, investigating the effect of the nitrogen protecting group and the relative configuration of the leaving group at C3 and C4 on the outcome of this reaction. We have observed that the sodium hydride-promoted heterocyclization of alkyl N-(cis-3,trans-4-dibromocyclohex-1-yl)carbamates (10, 12, 14, 16, 18) is a convenient method for the synthesis of 7-azabicyclo[2.2.1]heptane derivatives. For instance, the reaction of tert-butyl N-(cis-3,trans-4-dibromocyclohex-1-yl)carbamate (10) with sodium hydride in DMF at room temperature provides 2-bromo-7-[(tert-butoxy)carbonyl]-7-azabicyclo[2.2.1]heptane (2) (52% yield), whose t-BuOK-promoted hydrogen bromide elimination affords 7-[(tert-butoxy)carbonyl]-7-azabicyclo[2.2.1]hept-2-ene (31) in 78% yield, an intermediate in the total synthesis of epibatidine (1). However, the NaH/DMF-mediated heterocyclization of alkyl N-(trans-3,cis-4-dibromocyclohex-1-yl)carbamates (11, 13) is a more structure dependent reaction, where the nucleophilic attack of the oxygen atom of the protecting group controls the outcome of the reaction, giving rise to benzooxazolone and 2-oxa-4-azabicyclo[3.3.1]non-3-ene derivatives, respectively, from low to moderate yields, in complex reaction mixtures. Conversely, the NaH/DMF heterocyclizations of N-(cis-3,trans-4-dibromocyclohex-1-yl)-2,2,2-trifluoroacetamide (40) or N-(trans-3,cis-4-dibromocyclohex-1-yl)-2,2,2-trifluoroacetamide (42) are very clean reactions giving 7-azabicyclo[2.2.1]heptane or 2-oxa-4-azabicyclo[3.3.1]non-3-ene derivatives, respectively, in good yields. Finally, a mechanistic investigation, based on DFT calculations, has been carried out to rationalize the formation of the different adducts.

  19. 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)44H2O (H2DSPTP=4'-(2,4-disulfophenyl)-3,2':6'3"-terpyridine, 1 and 2), {[Ni(DSPTP)(H2O)43H2O}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)22H2O}n (7), {[Cd(DSPTP)(H2O)22H2O}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

  20. 4-Halo-1,3-oxazoles: Unambiguous structural assignment of 2-halo-2-benzoyl-2 H-azirine-3-carboxylates thermal ring expansion products

    NASA Astrophysics Data System (ADS)

    Lopes, Susy; Nunes, Cláudio M.; Fausto, Rui; Melo, Teresa M. V. D. Pinho e.

    2009-02-01

    IR spectroscopy in cryogenic argon matrix of methyl 4-chloro-5-phenyl-1,3-oxazole-2-carboxylate and methyl 4-chloro-5-phenylisoxazole-3-carboxylate was applied for the structural assignment of these isomeric heterocycles. It was demonstrated that methyl 2-benzoyl-2-halo-2 H-azirine-3-carboxylates undergo thermal ring expansion to give 4-halo-5-phenyl-1,3-oxazole-2-carboxylates and not the isomeric isoxazoles.

  1. Cd(II) complexes with different nuclearity and dimensionality based on 3-hydrazino-4-amino-1,2,4-triazole

    SciTech Connect

    Xu, Cai-Xia; Zhang, Jian-Guo Yin, Xin; Jin, Xin; Li, Tong; Zhang, Tong-Lai; Zhou, Zun-Ning

    2015-03-15

    A series of zero- to two-dimensional Cd(II) coordination compounds have been synthesized by the reaction of Cd(II) salts and 3-hydrazino-4-amino-1,2,4-triazole di-hydrochloride (HATr·2HCl). [CdCl{sub 2}(HATr){sub 2}] (1) and [Cd{sub 2}Cl{sub 4}(HATr){sub 2}(H{sub 2}O){sub 2}] (2) have discrete mononuclear and binuclear structures, respectively. [Cd(HATr){sub 2}(ClO{sub 4}){sub 2}]{sub n} (3) presents polymeric 1-D chain and [Cd{sub 2}(NO{sub 3}){sub 2}Cl{sub 2}(HATr){sub 2}]{sub n} (4) shows 2-D frameworks. All Cd(II) ions exhibit distorted octahedral configurations in 1–3, whilst both hexa and heptacoordinated Cd(II) are formed in 4. The HATr ligands adopt chelating coordinated mode in 1, while tri-dentate bridging–chelating mode in 24. The chloride ion is a mono-coordinated ligand in 1 and 2, but it bridges two adjacent metal ions in 4. Furthermore, thermal behaviors have been investigated and the results reveal that all complexes have good thermal stability. The impact sensitivity test indicates that complex 3 is sensitive to impact stimuli. - Graphical abstract: Four Cd(II) complexes based on 3-hydrazino-4-amino-1,2,4-triazole ligands exhibit diverse structures from mononuclear to 2D networks. - Highlights: • Cd(II) complexes containing 3-hydrazino-4-amino-1,2,4-triazole ligands. • Mononuclear, binuclear, 1-D and 2-D structures. • Good thermal stability. • Thermal decomposition kinetics.

  2. Dihydropyridine Ca2+ channel antagonists and agonists block Kv4.2, Kv4.3 and Kv1.4 K+ channels expressed in HEK293 cells.

    PubMed

    Hatano, Noriyuki; Ohya, Susumu; Muraki, Katsuhiko; Giles, Wayne; Imaizumi, Yuji

    2003-06-01

    (1) We have determined the molecular basis of nicardipine-induced block of cardiac transient outward K(+) currents (I(to)). Inhibition of I(to) was studied using cloned voltage-dependent K(+) channels (Kv) channels, rat Kv4.3L, Kv4.2, and Kv1.4, expressed in human embryonic kidney cell line 293 (HEK293) cells. (2) Application of the dihydropyridine Ca(2+) channel antagonist, nicardipine, accelerated the inactivation rate and reduced the peak amplitude of Kv4.3L currents in a concentration-dependent manner (IC(50): 0.42 micro M). The dihydropyridine (DHP) Ca(2+) channel agonist, Bay K 8644, also blocked this K(+) current (IC(50): 1.74 micro M). (3) Nicardipine (1 micro M) slightly, but significantly, shifted the voltage dependence of activation and steady-state inactivation to more negative potentials, and also slowed markedly the recovery from inactivation of Kv4.3L currents. (4) Coexpression of K(+) channel-interacting protein 2 (KChIP2) significantly slowed the inactivation of Kv4.3L currents as expected. However, the features of DHP-induced block of K(+) current were not substantially altered. (5) Nicardipine exhibited similar block of Kv1.4 and Kv4.2 channels stably expressed in HEK293 cells; IC(50)'s were 0.80 and 0.62 micro M, respectively. (6) Thus, at submicromolar concentrations, DHP Ca(2+) antagonist and agonist inhibit Kv4.3L and have similar inhibiting effects on other components of cardiac I(to), Kv4.2 and Kv1.4.

  3. Vibrational spectroscopic characterization of the phosphate mineral kulanite Ba(Fe2+,Mn2+,Mg)2(Al,Fe3+)2(PO4)3(OH)3

    NASA Astrophysics Data System (ADS)

    Frost, Ray L.; López, Andrés; Xi, Yunfei; Granja, Amanda; Scholz, Ricardo

    2013-11-01

    The mineral kulanite BaFe2Al2(PO4)3(OH)3, a barium iron aluminum phosphate, has been studied by using a combination of electron microscopy and vibrational spectroscopy. Scanning electron microscopy with EDX shows the mineral is homogenous with no other phases present. The Raman spectrum is dominated by an intense band at 1022 cm-1 assigned to the PO43- ν1 symmetric stretching mode. Low intensity Raman bands at 1076, 1110, 1146, 1182 cm-1 are attributed to the PO43 - ν3 antisymmetric stretching vibrations. The infrared spectrum shows a complex spectral profile with overlapping bands. Multiple phosphate bending vibrations supports the concept of a reduction in symmetry of the phosphate anion. Raman spectrum at 3211, 3513 and 3533 cm-1 are assigned to the stretching vibrations of the OH units. Vibrational spectroscopy enables aspects on the molecular structure of kulanite to be assessed.

  4. (4E)-dehydrocitrals [(2E,4E)- and (2Z,4E )-3,7-dimethyl-2,4,6-octatrienals] from acarid mite Histiogaster sp. A096 (Acari: Acaridae).

    PubMed

    Hiraoka, H; Mori, N; Nishida, R; Kuwahara, Y

    2001-12-01

    A mixture of two monoterpenes was obtained as the opisthonotal gland secretion from unidentified Histiogaster sp. A096 (Acari: Acaridae), and their structures were elucidated to be (4E)-dehydrocitrals [(2E,4E)- and (2Z,4E)-3,7-dimethyl-2,4,6-octatrienals] by GC/MS, GC/FT-IR, UV and 1H-NMR spectra. Both isomers of (4E)-dehydrocitral prepared by syntheses in 4 steps from 3-methyl-2-butenal with 34.2% yields (based on the ylide) were separated by column chromatography into the (2E,4E)- and (2Z,4E)-3,7-dimethyl-2,4,6-octatrienal. Mass spectra together with GC retention times of the purified natural (4E)-dehydrocitrals were identical with those of synthetic (2E,4E)-3,7-dimethyl-2,4,6-octatrienal and (2Z,4E)-3,7-dimethyl-2,4,6-octatrienal. The geometry at the 2-C position of both synthetic (4E)-dehydrocitrals was confirmed by NOESY analyses. This is the first identification of (4E)-dehydrocitrals from the animal kingdom.

  5. Anisotropic laser properties of Yb:Ca3La2(BO3)4 disordered crystal

    NASA Astrophysics Data System (ADS)

    Wang, Lisha; Xu, Honghao; Pan, Zhongben; Han, Wenjuan; Chen, Xiaowen; Liu, Junhai; Yu, Haohai; Zhang, Huaijin

    2016-08-01

    A study is carried out experimentally on the anisotropy in the laser action of Yb:Ca3La2(BO3)4 disordered crystal, demonstrated with the output coupling changed over a wide range from 0.5% to 40%. Complex polarization state variation with output coupling and evolution with pump power are observed in the laser operation achieved with a- and c-cut crystal samples. A maximum output power of 8.2 W is produced at wavelengths around 1043 nm, with an incident pump power of 24.9 W, the optical-to-optical efficiency being 33%. The polarized absorption and emission cross section spectra are also presented.

  6. Crystal structure of Pb3(IO4(OH)2)2.

    PubMed

    Weil, Matthias

    2014-07-01

    The structure of the title compound, trilead(II) bis-[di-hydroxido-tetra-oxido-iodate(VII)], was determined from a crystal twinned by non-merohedry with two twin domains present [twin fraction 0.73 (1):0.27 (1)]. It contains three Pb(2+) cations and two IO4(OH)2 (3-) anions in the asymmetric unit. Each of the Pb(2+) cations is surrounded by eight O atoms (cut-off value = 3.1 Å) in the form of a distorted polyhedron. The octa-hedral IO4(OH)2 (3-) anions are arranged in rows extending parallel to [021], forming a distorted hexa-gonal rod packing. The cations and anions are linked into a framework structure. Although H-atom positions could not be located, O⋯O distances suggest medium-strength hydrogen-bonding inter-actions between the IO4(OH)2 octa-hedra, further consolidating the crystal packing.

  7. Crystal structure of Pb3(IO4(OH)2)2

    PubMed Central

    Weil, Matthias

    2014-01-01

    The structure of the title compound, trilead(II) bis­[di­hydroxido­tetra­oxido­iodate(VII)], was determined from a crystal twinned by non-merohedry with two twin domains present [twin fraction 0.73 (1):0.27 (1)]. It contains three Pb2+ cations and two IO4(OH)2 3− anions in the asymmetric unit. Each of the Pb2+ cations is surrounded by eight O atoms (cut-off value = 3.1 Å) in the form of a distorted polyhedron. The octa­hedral IO4(OH)2 3− anions are arranged in rows extending parallel to [021], forming a distorted hexa­gonal rod packing. The cations and anions are linked into a framework structure. Although H-atom positions could not be located, O⋯O distances suggest medium-strength hydrogen-bonding inter­actions between the IO4(OH)2 octa­hedra, further consolidating the crystal packing. PMID:25161496

  8. Enhanced dechlorination of 2,4-dichlorophenol by recoverable Ni/Fe-Fe3O4 nanocomposites.

    PubMed

    Xu, Cancan; Liu, Rui; Chen, Lvjun; Tang, Jialu

    2016-10-01

    Ni/Fe-Fe3O4 nanocomposites were synthesized for dechlorination of 2,4-dichlorophenol (2,4-DCP). The effects of the Ni content in Ni/Fe-Fe3O4 nanocomposites, solution pH, and common dissolved ions on the dechlorination efficiency were investigated, in addition to the reusability of the nanocomposites. The results showed that increasing content of Ni in Ni/Fe-Fe3O4 nanocomposites, from 1 to 5wt.%, greatly increased the dechlorination efficiency; the Ni/Fe-Fe3O4 nanocomposites had much higher dechlorination efficiency than bare Ni/Fe nanoparticles. Ni content of 5wt.% and initial pH below 6.0 was found to be the optimal conditions for the catalytic dechlorination of 2,4-DCP. Both 2,4-DCP and the intermediate product 2-chlorophenol (2-CP) were completely removed, and the concentration of the final product phenol was close to the theoretical phenol production from complete dechlorination of 20mg/L of 2,4-DCP, after 3hr reaction at initial pH value of 6.0, 3g/L Ni/Fe-Fe3O4, 5wt.% Ni content in the composite, and temperature of 22°C. 2,4-DCP dechlorination was enhanced by Cl(-) and inhibited by NO3(-) and SO4(2-). The nanocomposites were easily separated from the solution by an applied magnetic field. When the catalyst was reused, the removal efficiency of 2,4-DCP was almost 100% for the first seven uses, and gradually decreased to 75% in cycles 8-10. Therefore, the Ni/Fe-Fe3O4 nanocomposites can be considered as a potentially effective tool for remediation of pollution by 2,4-DCP.

  9. Mass spectrum of the 1-butene-3-yne-2-yl radical (i-C4H3; X2A')

    NASA Astrophysics Data System (ADS)

    Guo, Ying; Gu, Xibin; Kaiser, Ralf I.

    2006-03-01

    The crossed molecular beams method has been applied to produce the 1-butene-3-yne-2-yl radical, i-C4H3(X2A') under single collision conditions via the reaction of dicarbon molecules with ethylene. We recorded time-of-flight spectra of the radical at the center-of-mass angle (28.0°) of the parent ion (m/z = 51; C4H3+) and of the fragments at m/z = 50 (C4H2+), m/z = 49 (C4H+), m/z = 48 (C4+), m/z = 39 (C3H3+), m/z = 38 (C3H2+), m/z = 37 (C3H+), and m/z = 36 (C3+). This yielded relative intensity ratios of I(m/z = 51):I(m/z = 50):I(m/z = 49):I(m/z = 48):I(m/z = 39):I(m/z = 38):I(m/z = 37):I(m/z = 36) = 0.47 +/- 0.01:0.94 +/- 0.01:1.0:0.07 +/- 0.02:0.31 +/- 0.01:0.23 +/- 0.02:0.24 +/- 0.01:0.12 +/- 0.01 at 70 eV electron impact energy. Upper limits at mass-to-charge ratios between 27 and m/z = 24 and m/z = 14-12 were derived to be 0.02 +/- 0.01. Note that the intensity of the 13C isotopic peak of the 1-butene-3-yne-2-yl radical at m/z = 52 (13C12C3H3+) is about 0.04 +/- 0.01 relative to m/z = 51. Employing linear scaling methods, the absolute electron impact ionization cross section of the 1-butene-3-yne-2-yl radical was computed to be 7.8 +/- 1.6 × 10-16 cm2. These data can be employed to monitor the 1-butene-3-yne-2-yl radical in oxygen-poor combustion flames and in the framework of prospective explorations of planetary atmospheres (Jupiter, Saturn, Uranus, Neptune, Pluto) and of their moons (Titan, Triton, Oberon) in situ via matrix interval arithmetic assisted mass spectrometry.

  10. 40 CFR 721.10162 - 1,3 Dioxolane-4-butanol, 2-ethenyl-.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false 1,3 Dioxolane-4-butanol, 2-ethenyl... Specific Chemical Substances § 721.10162 1,3 Dioxolane-4-butanol, 2-ethenyl-. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 1,3 dioxolane-4-butanol,...

  11. 40 CFR 721.10162 - 1,3 Dioxolane-4-butanol, 2-ethenyl-.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 31 2011-07-01 2011-07-01 false 1,3 Dioxolane-4-butanol, 2-ethenyl... Specific Chemical Substances § 721.10162 1,3 Dioxolane-4-butanol, 2-ethenyl-. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 1,3 dioxolane-4-butanol,...

  12. 40 CFR 721.10162 - 1,3 Dioxolane-4-butanol, 2-ethenyl-.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 32 2012-07-01 2012-07-01 false 1,3 Dioxolane-4-butanol, 2-ethenyl... Specific Chemical Substances § 721.10162 1,3 Dioxolane-4-butanol, 2-ethenyl-. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 1,3 dioxolane-4-butanol,...

  13. 40 CFR 721.10162 - 1,3 Dioxolane-4-butanol, 2-ethenyl-.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false 1,3 Dioxolane-4-butanol, 2-ethenyl... Specific Chemical Substances § 721.10162 1,3 Dioxolane-4-butanol, 2-ethenyl-. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 1,3 dioxolane-4-butanol,...

  14. 40 CFR 721.10162 - 1,3 Dioxolane-4-butanol, 2-ethenyl-.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 32 2013-07-01 2013-07-01 false 1,3 Dioxolane-4-butanol, 2-ethenyl... Specific Chemical Substances § 721.10162 1,3 Dioxolane-4-butanol, 2-ethenyl-. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 1,3 dioxolane-4-butanol,...

  15. Silica gel-catalyzed one-pot syntheses in water and fluorescence properties studies of 5-amino-2-aryl-3H-chromeno[4,3,2-de][1,6]naphthyridine-4-carbonitriles and 5-amino-2-aryl-3H-quinolino[4,3,2-de][1,6]naphthyridine-4-carbonitriles.

    PubMed

    Wu, Hui; Lin, Wei; Wan, Yu; Xin, Hai-qiang; Shi, Da-qing; Shi, Yan-hui; Yuan, Rui; Bo, Rong-cheng; Yin, Wei

    2010-01-01

    The silica gel-catalyzed synthesis of 5-amino-2-aryl-3H-chromeno[4,3,2-de][1,6]naphthyridine-4-carbonitriles and 5-amino-2-aryl-3H-quinolino[4,3,2-de][1,6]naphthyridine-4-carbonitriles were simply achieved upon the one-pot cascade reaction of malononitrile with substituted 2-hydroxyacetophenone (or 2-aminoacetophenone) and aromatic aldehyde in aqueous media. The mechanistic investigation results based on electrospray ionization mass spectrometry (ESI-MS) indicated that malononitrile displayed a dual role during this transformation. Thirteen bonds were cleaved and 12 new bonds were constructed in the formation of 5-amino-2-aryl-3H-chromeno[4,3,2-de][1,6]naphthyridine-4-carbonitriles, while only 2 H(2)O molecules were removed. The fluorescence properties screening showed five new compounds have high fluorescence quantum yields.

  16. 2-Chloro-methyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine.

    PubMed

    Xu, Jian; Xu, Hao; Quan, Ji-Cai; Sha, Fei; Yao, Cheng

    2009-03-06

    In the mol-ecule of the title compound, C(7)H(7)ClO(2)S, the six-membered ring adopts a twisted conformation. In the crystal structure, weak inter-molecular C-H⋯O hydrogen bonds link the mol-ecules. There is also a weak C-H⋯π inter-action.

  17. Site occupation and photoluminescence properties of Ce3+ in Sr4Ca4La2 (PO4)6O2: Experiments and ab initio calculations

    NASA Astrophysics Data System (ADS)

    Zhou, Rongfu; Ning, Lixin; Zhou, Weijie; Lin, Litian; Shi, Rui; Liang, Hongbin

    2017-04-01

    Cerium-doped oxyapatite phosphors, Sr4Ca4La2(PO4)6O2: Ce3+, are prepared by a traditional solid-state reaction method. X-ray diffraction (XRD) refinement reveals that the hexagonal Sr4Ca4La2(PO4)6O2 structure is characterized by a random distribution of Sr and Ca atoms on the nine-coordinated cationic 4f sites and of Sr, Ca, and La atoms on the seven-coordinated cationic 6 h sites. Photoluminescence properties of Ce-doped samples are then studied with excitation energies in the vacuum-ultraviolet (VUV) to ultraviolet (UV) range at low temperature. Three main types of occupation sites for Ce3+ are identified based on analysis of emission and excitation spectra and of luminescence decay behaviors. The Ce3+ occupation on the seven-coordinated La (6 h) site is found to be dominant, which is supported by wave function-based CASSCF/CASPT2 embedded cluster calculations on Ce3+ 4f → 5d transition energies at the spin-orbit level. The role of the coordinated oxygen ion that is not bonded with P5+ in the 5d centroid shift of CeLa(6h)3+ is emphasized. The thermal stability and doping concentration dependence of the 5d luminescence are also investigated and discussed in association with the coordination structures of Ce3+.

  18. Hygroscopic Properties of CH3SO3Na, CH3SO3NH4, (CH3SO3)2Mg and (CH3SO3)2Ca Particles Studied by Micro-FTIR Spectroscopy

    SciTech Connect

    Liu, Yong; Laskin, Alexander

    2009-02-26

    The hygroscopic behavior of CH3SO3Na, CH3SO3NH4, (CH3SO3)2Mg and (CH3SO3)2Ca particles as a function of relative humidity (RH) has been studied using microscopic Fourier transform infrared (micro-FTIR) spectroscopy. The approach used exposure of substrate deposited, ~1 μm dry-size particles to humidified nitrogen followed by micro-FTIR spectroscopy over a selected sample area. The results show that CH3SO3Na particles undergo characteristic phase transitions at deliquescence relative humidity (DRH) of 71% and efflorescence relative humidity (ERH) of ~40%. In contrast, CH3SO3NH4, (CH3SO3)2Mg and (CH3SO3)2Ca particles do not undergo phase transitions and exhibit continuous, reversible uptake and evaporation of water under the influence of changing RH. The extent of water uptake is quantified and presented as water-to-solute ratios (WSR) in particles as a function of RH. The WSR values are determined from the integrated absorbance of the water and the solute-specific bands in IR spectra recorded at different RH.

  19. Optimization of a Novel Binding Motif to (E)-3-(3,5-Difluoro-4-((1R,3R)-2-(2-fluoro-2-methylpropyl)-3-methyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indol-1-yl)phenyl)acrylic Acid (AZD9496), a Potent and Orally Bioavailable Selective Estrogen Receptor Downregulator and Antagonist.

    PubMed

    De Savi, Chris; Bradbury, Robert H; Rabow, Alfred A; Norman, Richard A; de Almeida, Camila; Andrews, David M; Ballard, Peter; Buttar, David; Callis, Rowena J; Currie, Gordon S; Curwen, Jon O; Davies, Chris D; Donald, Craig S; Feron, Lyman J L; Gingell, Helen; Glossop, Steven C; Hayter, Barry R; Hussain, Syeed; Karoutchi, Galith; Lamont, Scott G; MacFaul, Philip; Moss, Thomas A; Pearson, Stuart E; Tonge, Michael; Walker, Graeme E; Weir, Hazel M; Wilson, Zena

    2015-10-22

    The discovery of an orally bioavailable selective estrogen receptor downregulator (SERD) with equivalent potency and preclinical pharmacology to the intramuscular SERD fulvestrant is described. A directed screen identified the 1-aryl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole motif as a novel, druglike ER ligand. Aided by crystal structures of novel ligands bound to an ER construct, medicinal chemistry iterations led to (E)-3-(3,5-difluoro-4-((1R,3R)-2-(2-fluoro-2-methylpropyl)-3-methyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indol-1-yl)phenyl)acrylic acid (30b, AZD9496), a clinical candidate with high oral bioavailability across preclinical species that is currently being evaluated in phase I clinical trials for the treatment of advanced estrogen receptor (ER) positive breast cancer.

  20. Electroreductive Intermolecular Coupling of Coumarins with Benzophenones: Synthesis of 4-(2-Hydroxyphenyl)-5,5-diaryl-γ-butyrolactones, 2-(2,2-Diaryl-2,3-dihydrobenzofuran-3-yl)acetic Acids, and 4-(Diarylmethyl)coumarins.

    PubMed

    Kise, Naoki; Hamada, Yusuke; Sakurai, Toshihiko

    2016-11-18

    The electroreductive coupling of coumarins with benzophenones in the presence of TMSCl gave adducts reacted at the 4-position of coumarins as trimethylsilyl ethers. From 3-methylcoumarin, 3,4-cis-adducts were formed stereoselectively. The de-trimethylsilylation of the adducts with 1 M HCl aq or TBAF in THF at 25 °C produced 4-(2-hydroxyphenyl)-5,5-diaryl-γ-butyrolactones. The γ-butyrolactones were further transformed to 2-(2,2-diaryl-2,3-dihydrobenzofuran-3-yl)acetic acids by treatment with 1 M HCl aq at reflux temperature. The de-trimethylsilylation of the adducts with 1 M HCl in MeOH afforded 2-(2,2-diaryl-2,3-dihydrobenzofuran-3-yl)acetic acid methyl esters. The de-trimethylsiloxylation of the adducts or dehydration of the γ-butyrolactones brought about 4-(diarylmethyl)coumarins.

  1. Crystal structure of rac-2,3-diphenyl-2,3,5,6-tetrahydro-4H-1,3-thiazin-4-one 1-oxide

    PubMed Central

    Yennawar, Hemant P.; Yang, Ziwei; Silverberg, Lee J.

    2016-01-01

    In the title compound, C16H15NO2S [alternative name: rac-2,3-diphenyl-1,3-thia­zinan-4-one 1-oxide], the thia­zine ring exhibits an envelope conformation, with the S atom forming the flap. The sulfoxide O atom is in a pseudo-axial position on the thia­zine ring and is trans to the phenyl group on C-2. The phenyl rings form a dihedral angle of 89.47 (19)°. In this racemate crystal, homochiral mol­ecules form slabs parallel to (010) of thickness b/2 which then stack with alternating chirality in the b-axis direction. The stacking is aided by edge-to-face inter­actions between the phenyl rings of racemic mol­ecules. Within each of the single-enanti­omer slabs, the mol­ecules are held by C—H⋯O-type inter­actions, with an H⋯O distance of 2.30 Å, forming infinite chains along the c-axis direction, as well by the edge-to-face inter­actions between phenyl rings of neighboring mol­ecules in the a-axis direction. PMID:27840703

  2. Mixed-metal uranium(VI) iodates: hydrothermal syntheses, structures, and reactivity of Rb[UO(2)(CrO(4))(IO(3))(H(2)O)], A(2)[UO(2)(CrO(4))(IO(3))(2)] (A = K, Rb, Cs), and K(2)[UO(2)(MoO(4))(IO(3))(2)].

    PubMed

    Sykora, Richard E; McDaniel, Steven M; Wells, Daniel M; Albrecht-Schmitt, Thomas E

    2002-10-07

    The reactions of the molecular transition metal iodates A[CrO(3)(IO(3))] (A = K, Rb, Cs) with UO(3) under mild hydrothermal conditions provide access to four new, one-dimensional, uranyl chromatoiodates, Rb[UO(2)(CrO(4))(IO(3))(H(2)O)] (1) and A(2)[UO(2)(CrO(4))(IO(3))(2)] (A = K (2), Rb (3), Cs (4)). Under basic conditions, MoO(3), UO(3), and KIO(4) can be reacted to form K(2)[UO(2)(MoO(4))(IO(3))(2)] (5), which is isostructural with 2 and 3. The structure of 1 consists of one-dimensional[UO(2)(CrO(4))(IO(3))(H(2)O)](-) ribbons that contain uranyl moieties bound by bridging chromate and iodate anions as well as a terminal water molecule to create [UO(7)] pentagonal bipyramidal environments around the U(VI) centers. These ribbons are separated from one another by Rb(+) cations. When the iodate content is increased in the hydrothermal reactions, the terminal water molecule is replaced by a monodentate iodate anion to yield 2-4. These ribbons can be further modified by replacing tetrahedral chromate anions with MoO(4)(2)(-) anions to yield isostructural, one-dimensional [UO(2)(MoO(4))(IO(3))(2)](2)(-) ribbons. Crystallographic data: 1, triclinic, space group P(-)1, a = 7.3133(5) A, b = 8.0561(6) A, c = 8.4870(6) A, alpha = 88.740(1) degrees, beta = 87.075(1) degrees, gamma = 71.672(1) degrees, Z = 2; 2, monoclinic, space group P2(1)/c, a = 11.1337(5) A, b = 7.2884(4) A, c = 15.5661(7) A, beta = 107.977(1) degrees, Z = 4; 3, monoclinic, space group P2(1)/c, a = 11.3463(6) A, b = 7.3263(4) A, c = 15.9332(8) A, beta = 108.173(1) degrees, Z = 4; 4, monoclinic, space group P2(1)/n, a = 7.3929(5) A, b = 8.1346(6) A, c = 22.126(2) A, beta = 90.647(1) degrees, Z = 4; 5, monoclinic, space group P2(1)/c, a = 11.3717(6) A, b = 7.2903(4) A, c = 15.7122(8) A, beta = 108.167(1) degrees, Z = 4.

  3. Electronic structure and properties of Cd4As2Br3 and Cd4Sb2I3, analogues of CdSe and CdTe

    NASA Astrophysics Data System (ADS)

    Roy, Anand; Suchitra; Manjunath, K.; Ahmad, Tokeer; Waghmare, Umesh V.; Rao, C. N. R.

    2017-04-01

    Substitution of aliovalent anions in metal oxides and chalcogenides significantly affects the electronic structure and properties of the materials. Thus, substitution of P3- and Cl- in CdS decreases the band gap and favorably influences the photocatalytic activity. Complete substitution of a trivalent (A3-) and a monovalent (B-) anions in a cadmium chalcogenides, CdX, should give rise to a material of the composition Cd A0.5B0.5 or Cd2AB, but a compound with the composition Cd4P2Cl3 (or Cd2PCl1.5) is obtained in the case of CdS. We have investigated the analogous compounds, Cd4As2Br3 and Cd4Sb2I3, wherein the anions in CdSe and CdTe are substituted by As, Br and Sb, I respectively. These compounds are direct band gap semiconductors with a band gap of 1.8-1.9 eV and a photoluminescence band in the visible region. First-principles calculations show both Cd4As2Br3 and Cd4Sb2I3 to be direct band gap semiconductors. The arsenic bromide is predicted to be photochemically more active for HER than the antimony iodide.

  4. Bi2O(XO4)(IO3)2 (X = S, Se, Cr): Three-dimensional frameworks containing [Bi4O2]8+ clusters

    NASA Astrophysics Data System (ADS)

    Shi, Long; Mei, Dajiang; Xu, Jingli; Wu, Yuandong

    2017-01-01

    Three new bismuth-based compounds, Bi2O(XO4)(IO3)2 (X = S, Se, Cr) have been synthesized by hydrothermal method and characterized by single-crystal X-ray diffraction. Title compounds crystallize in the monoclinic space group P21/n (No.14) with lattice parameters: a = 7.2391(5), b = 17.9074(12), c = 7.7964(5) Å, β = 109.6521(15) °, Z = 4 for Bi2O(SO4)(IO3)2; a = 7.2665(4), b = 18.0115(10), c = 7.9310(5) Å, β = 109.7480(10) °, Z = 4 for Bi2O(SeO4)(IO3)2; and a = 7.2708(6), b = 17.9967(14), c = 7.8998(6) Å, β = 109.799(2) °, Z = 4 for Bi2O(CrO4)(IO3)2, respectively. All compounds exhibit three-dimensional frameworks that are composed of [Bi4O2]8+ clusters, [IO3]- and [XO4]2- (X = S, Se, Cr) groups. Bi atoms occur in two different coordination types, showing the stereochemical influence of the Bi3+ lone electron pair. Title compounds were characterized by infrared spectra, solid state UV-vis-NIR diffuse reflectance spectroscopy and thermogravimetric analysis.

  5. CH3Cl, CH2Cl2, CHCl3, and CCl4: Infrared spectra, radiative efficiencies, and global warming potentials

    NASA Astrophysics Data System (ADS)

    Wallington, Timothy J.; Pivesso, Bruno Pasquini; Lira, Alane Moura; Anderson, James E.; Nielsen, Claus Jørgen; Andersen, Niels Højmark; Hodnebrog, Øivind

    2016-05-01

    Infrared spectra for the title compounds were measured experimentally in 700 Torr of air at 295 K and systematically modeled in B3LYP, M06-2X and MP2 calculations employing various basis sets. Calibrated infrared spectra over the wavenumber range 600-3500 cm-1 are reported and combined with literature data to provide spectra for use in experimental studies and radiative transfer calculations. Integrated absorption cross sections are (units of cm-1 molecule-1): CH3Cl, 660-780 cm-1, (3.89±0.19)×10-18; CH2Cl2, 650-800 cm-1, (2.16±0.11)×10-17; CHCl3, 720-810 cm-1, (4.08±0.20)×10-17; and CCl4, 730-825 cm-1, (6.30±0.31)×10-17. CH3Cl, CH2Cl2, CHCl3, and CCl4 have radiative efficiencies of 0.004, 0.028, 0.070, and 0.174 W m-2 ppb-1 and global warming potentials (100 year horizon) of 5, 8, 15, and 1775, respectively. Quantum chemistry calculations generally predict larger band intensities than the experimental values. The best agreement with experiments is obtained in MP2(Full) calculations employing basis sets of at least triple-zeta quality augmented by diffuse functions. The B3LYP functional is found ill-suited for calculating vibrational frequencies and infrared intensities of halocarbons.

  6. Synthesis of isomeric isothiazolo[4',3':4,5]- and isothiazolo[4',5':4,5]thieno[3,2-b]pyrano[2,3-d]pyridines by combination of domino reactions.

    PubMed

    Shestopalov, Anatoliy M; Larionova, Natalia A; Fedorov, Alexander E; Rodinovskaya, Lyudmila A; Mortikov, Valery Yu; Zubarev, Andrey A; Bushmarinov, Ivan S

    2013-10-14

    Isothiazolothienopyridines have been prepared by a domino reaction (the SN2 reaction → the Thorpe-Ziegler reaction → the Thorpe-Guareschi reaction type) from disodium 4-cyanoisothiazole-3,5-dithiolate. By changing the order of addition of the alkylation reagents in the reaction with disodium 4-cyanoisothiazole-3,5-dithiolate both possible isomers of the isothiazolothienopyridines are synthesized. These isomers were further used in three-component domino reaction (the Knoevenagel reaction → the Michael reaction → the hetero-Thorpe-Ziegler reaction type) to obtain wide range of isomeric isothiazolothienopyranopyridines.

  7. 4-Benzoyl-3,4-dihydro-2H-1,4-benzoxazine-2-carbonitrile: refinement using a multipolar atom model.

    PubMed

    Ejsmont, Krzysztof; Joly, Jean Pierre; Wenger, Emmanuel; Guillot, Benoit; Jelsch, Christian

    2009-07-01

    The structural model for the title compound, C(16)H(12)N(2)O(2), was refined using a multipolar atom model transferred from an experimental electron-density database. The refinement showed some improvements of crystallographic statistical indices when compared with a conventional spherical neutral-atom refinement. The title compound adopts a half-chair conformation. The amide N atom lies almost in the plane defined by the three neighbouring C atoms. In the crystal structure, molecules are linked by weak intermolecular C-H...O and C-H...pi hydrogen bonds.

  8. 40 CFR 721.5260 - 1,3,6-Naphthalenetrisulfonic acid, 7-[[2-[(aminocarbonyl)amino]- 4-[[4-[[2-[2-(ethenylsulfonyl...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ...,3,6-Naphthalenetrisulfonic acid, 7- - 4- ethyl]amino]- 6-fluoro-1,3,5-triazin-2-yl]amino]phenyl]azo... substance identified as 1,3,6-Naphthalenetrisulfonic acid, 7- -4- ethyl]amino]-6-fluoro-1,3,5-triazin-2-yl... 40 Protection of Environment 32 2012-07-01 2012-07-01 false 1,3,6-Naphthalenetrisulfonic acid,...

  9. 40 CFR 721.5260 - 1,3,6-Naphthalenetrisulfonic acid, 7-[[2-[(aminocarbonyl)amino]- 4-[[4-[[2-[2-(ethenylsulfonyl...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ...,3,6-Naphthalenetrisulfonic acid, 7- - 4- ethyl]amino]- 6-fluoro-1,3,5-triazin-2-yl]amino]phenyl]azo... substance identified as 1,3,6-Naphthalenetrisulfonic acid, 7- -4- ethyl]amino]-6-fluoro-1,3,5-triazin-2-yl... 40 Protection of Environment 31 2014-07-01 2014-07-01 false 1,3,6-Naphthalenetrisulfonic acid,...

  10. 40 CFR 721.5260 - 1,3,6-Naphthalenetrisulfonic acid, 7-[[2-[(aminocarbonyl)amino]- 4-[[4-[[2-[2-(ethenylsulfonyl...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ...,3,6-Naphthalenetrisulfonic acid, 7- - 4- ethyl]amino]- 6-fluoro-1,3,5-triazin-2-yl]amino]phenyl]azo... substance identified as 1,3,6-Naphthalenetrisulfonic acid, 7- -4- ethyl]amino]-6-fluoro-1,3,5-triazin-2-yl... 40 Protection of Environment 32 2013-07-01 2013-07-01 false 1,3,6-Naphthalenetrisulfonic acid,...

  11. 40 CFR 721.5260 - 1,3,6-Naphthalenetrisulfonic acid, 7-[[2-[(aminocarbonyl)amino]- 4-[[4-[[2-[2-(ethenylsulfonyl...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...,3,6-Naphthalenetrisulfonic acid, 7- - 4- ethyl]amino]- 6-fluoro-1,3,5-triazin-2-yl]amino]phenyl]azo... substance identified as 1,3,6-Naphthalenetrisulfonic acid, 7- -4- ethyl]amino]-6-fluoro-1,3,5-triazin-2-yl... 40 Protection of Environment 30 2010-07-01 2010-07-01 false 1,3,6-Naphthalenetrisulfonic acid,...

  12. 40 CFR 721.5260 - 1,3,6-Naphthalenetrisulfonic acid, 7-[[2-[(aminocarbonyl)amino]- 4-[[4-[[2-[2-(ethenylsulfonyl...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...,3,6-Naphthalenetrisulfonic acid, 7- - 4- ethyl]amino]- 6-fluoro-1,3,5-triazin-2-yl]amino]phenyl]azo... substance identified as 1,3,6-Naphthalenetrisulfonic acid, 7- -4- ethyl]amino]-6-fluoro-1,3,5-triazin-2-yl... 40 Protection of Environment 31 2011-07-01 2011-07-01 false 1,3,6-Naphthalenetrisulfonic acid,...

  13. Chanabayaite, Cu2(N3C2H2)Cl(NH3,Cl,H2O,□)4, a new mineral containing triazolate anion

    NASA Astrophysics Data System (ADS)

    Chukanov, N. V.; Zubkova, N. V.; Möhn, G.; Pekov, I. V.; Pushcharovsky, D. Yu.; Zadov, A. E.

    2015-12-01

    A new mineral, chanabayaite, has been discovered at a guano deposit located at Mt. Pabellón de Pica near the village of Chanabaya, Iquique Province, Tarapacá region, Chile. It is associated with salammoniac, halite, joanneumite, nitratine and earlier chalcopyrite. Chanabayaite occurs as blue translucent imperfect prismatic crystals, up to 0.05 × 0.1 × 0.5 mm in size, and their radial aggregates. Chanabayaite is brittle, with a Mohs' hardness of 2. The cleavage is perfect on (001) and imperfect on (100) and (010). D meas = 1.48(2) g/cm3, D calc = 1.464 g/cm3. The mineral is optically biaxial (-), α = 1.561(2), β = 1.615(3), γ = 1.620(2), 2 V meas = 25(10)°, 2 V calc = 33°. Pleochroism is strong, Z ≈ Y (deep blue) ≫ X (pale blue with gray tint). IR spectrum is given. The chemical composition (electron microprobe data for Cu, Fe and Cl; gas chromatography data for H, N, C and O) is as follows (wt %): 32.23 Cu, 1.14 Fe, 16.13 Cl, 3.1 H, 29.9 N, 12.2 C, 3.4 O, total is 98.1. The empirical formula is ( Z = 4): Cu1.92Fe0.08Cl1.72N8.09C3.85H11.66O0.81. The structural model was based on the single-crystal X-ray diffraction data ( R = 0.1627). Chanabayaite is orthorhombic, space group Imma, a = 19.484(3), b = 7.2136(10), c = 11.999(4) Å, V = 1686.5(7) Å3, Z = 2. In chanabayaite, chains of the corner-sharing Cu(l)-centered octahedra and single Cu(2)-centered octahedra are linked via 1,2,4-triazolate anions C2N3H2 -. NH3 and Cl- are additional ligands coordinating Cu2+. Chanabayaite is a transformational mineral species formed by leaching of Na and one third of Cl and partial dehydration of the protophase Na2Cu2Cl3(N3C2H2)2(NH3)24H2O. The strongest reflections in the powder X-ray diffraction pattern [ d, Å ( I, %) ( hkl)] are detected: 10.19 (100) (101), 6.189 (40) (011), 5.729 (23) (301), 5.216 (75) (211, 202), 4.964 (20) (400), 2.830 (20) (602, 413, 503), 2.611 (24) (123, 422, 404).

  14. Tetra-butyl-ammonium 2-[2,5-dimethyl-3-(4-nitro-phen-yl)-2,3-dihydro-1,2,4-oxadiazo-lium-4-yl]nona-hydro-closo-deca-borate.

    PubMed

    Mindich, Aleksey L; Pavlishchuk, Anna V; Bokach, Nadezhda A; Starova, Galina L; Zhizhin, Konstantin Yu

    2012-12-01

    The title ionic compound, C16H36N(+)·C10H20B10N3O3(-), consists of a tetra-butyl-ammonium cation and a closo-deca-borate cluster anion, which is bound to the substituted 2,3-dihydro-1,2,4-oxadiazole ring through a B-N bond [1.540 (2) Å]. The distances between connected B atoms in the deca-borate cluster range from 1.689 (2) to 1.844 (2) Å. The 2,3-dihydro-1,2,4-oxadiazole ring adopts an envelope conformation with the N atom as the flap atom.

  15. Nqrs Data for C6H16I2N4O8 [C6H14N4O2·2(HIO3)] (Subst. No. 0932)

    NASA Astrophysics Data System (ADS)

    Chihara, H.; Nakamura, N.

    This document is part of Subvolume A `Substances Containing Ag … C10H15' of Volume 48 `Nuclear Quadrupole Resonance Spectroscopy Data' of Landolt-Börnstein - Group III `Condensed Matter'. It contains an extract of Section `3.2 Data tables' of the Chapter `3 Nuclear quadrupole resonance data' providing the NQRS data for C6H16I2N4O8 [C6H14N4O2·2(HIO3)] (Subst. No. 0932)

  16. 3,3'- and 4,4'-Dimethoxy-2,2'-bipyrroles: highly electron-rich model compounds for polypyrrole formation.

    PubMed

    Merz, Andreas; Anikin, Sergiy; Lieser, Bernd; Heinze, Jürgen; John, Hermann

    2003-01-20

    3,3'-Dimethoxy-2,2'-bipyrrole (1) and 4,4'-dimethoxy-2,2'-bipyrrole (2) were obtained in short sequences and good yields from N-benzyl-3-hydroxypyrrole-2,4-dicarboxylic acid. The key intermediate leading to 1 is an N-benzyl-3-methoxypyrrole, which is dimerized by lithiation and oxidation with NiCl(2). The formation of 2 is achieved by a classical Ullmann coupling of diethyl 1-benzyl-2-bromo-4-methoxypyrrole-3,5-dicarboxylate. The N-benzyl protection groups of 1 and 2 are cleaved under reducing conditions with sodium in liquid ammonia. Both isomeric bipyrroles are extremely sensitive toward air. Compound 1 has a very low oxidation potential of 0.09 V against AgCl but film formation hardly occurs. On the other hand, compound 2 with a potential of 0.35 V readily forms stable polypyrrole films with anodic waves at -0.51 and -0.35 V and a cathodic wave at -0.77 V, the lowest potential ever observed for a p-doped polymer.

  17. 49 CFR 173.124 - Class 4, Divisions 4.1, 4.2 and 4.3-Definitions.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... exothermic decomposition even without participation of oxygen (air). A material is excluded from this...: (1) Its heat of decomposition is less than 300 J/g; or (2) Its self-accelerating decomposition... decomposition temperature is 50 °C (122 °F) or higher for a 50 kg (110 pounds) package). A...

  18. 49 CFR 173.124 - Class 4, Divisions 4.1, 4.2 and 4.3-Definitions.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... exothermic decomposition even without participation of oxygen (air). A material is excluded from this...: (1) Its heat of decomposition is less than 300 J/g; or (2) Its self-accelerating decomposition... decomposition temperature is 50 °C (122 °F) or higher for a 50 kg (110 pounds) package). A...

  19. 49 CFR 173.124 - Class 4, Divisions 4.1, 4.2 and 4.3-Definitions.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... exothermic decomposition even without participation of oxygen (air). A material is excluded from this...: (1) Its heat of decomposition is less than 300 J/g; or (2) Its self-accelerating decomposition... decomposition temperature is 50 °C (122 °F) or higher for a 50 kg (110 pounds) package). A...

  20. 49 CFR 173.124 - Class 4, Divisions 4.1, 4.2 and 4.3-Definitions.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... exothermic decomposition even without participation of oxygen (air). A material is excluded from this...: (1) Its heat of decomposition is less than 300 J/g; or (2) Its self-accelerating decomposition... decomposition temperature is 50 °C (122 °F) or higher for a 50 kg (110 pounds) package). A...

  1. 49 CFR 173.124 - Class 4, Divisions 4.1, 4.2 and 4.3-Definitions.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... exothermic decomposition even without participation of oxygen (air). A material is excluded from this...: (1) Its heat of decomposition is less than 300 J/g; or (2) Its self-accelerating decomposition... decomposition temperature is 50 °C (122 °F) or higher for a 50 kg (110 pounds) package). A...

  2. Fluorine-containing heterocycles: synthesis and some reactions of new 3-amino-2-functionalized-6-(2'-thienyl)-4-trifluoromethylthieno [2,3-b]pyridines.

    PubMed

    Abdel-Monem, M I; Mohamed, O S; Bakhite, E A

    2001-01-01

    3-Cyano-6-(2'-thienyl)-4-trifluoromethylpyridine-2(1H)-thione (2) was prepared and reacted with chloroacetone or phenacyl bromide to yield the 2-acetyl or benzoyl-3-amino-6-(2'-thienyl)-4-trifluoromethylthieno[2,3-b]pyridines (3a, b). In contrast, the reaction of 2 with chloroacetamide or its N-aryl derivatives gave the corresponding 2-carbamoylmethyl thiopyridines 4a-c. Upon treatment of these educts with K2CO3 or C2H5ONa in ethanol, they underwent intramolecular Thorpe-Ziegler cyclization to afford 3-amino-2-carbamoyl-6-(2'-thienyl)-4-trifluoromethyl-thieno[2,3-b]pyridine (5a) and its N-aryl analogs 5b, c. Compounds 5a-c underwent some reactions to yield new pyrido[3',2':4,5]thieno[3,2-d]pyrimidines and pyrido[3',2':4,5]thieno[3,2-d][1,2,3] triazines.

  3. 3,4-Dihydroxyphenylacetate 2,3-dioxygenase from Klebsiella pneumoniae, a Mg(2+)-containing dioxygenase involved in aromatic catabolism.

    PubMed Central

    Gibello, A; Ferrer, E; Martín, M; Garrido-Pertierra, A

    1994-01-01

    3,4-Dihydroxyphenylacetate 2,3-dioxygenase, an extradiol-ring-cleavage dioxygenase, has been purified from Klebsiella pneumoniae to homogeneity. The enzyme has an M(r) of 102,000 in its tetrameric form with an M(r) of 25,500 for each subunit. Unlike most other dioxygenases, the enzyme reported here contains Mg2+, as determined by atomic-absorption spectrophotometry and plasma emission metal analysis. The enzyme was shown to contain approx. 1 g-atom of Mg2+/mol of protein and we suggest an alpha 4 Mg2+ quaternary structure. This is the first report of a dioxygenase containing Mg2+ in its structure. Images Figure 1 PMID:8037662

  4. Crystal structures of four 1-(aryl)-[1,2,4]triazolo[4,3-a]quinoxaline derivatives

    NASA Astrophysics Data System (ADS)

    Nogueira, Thais C. M.; Pinheiro, Alessandra C.; de Souza, Marcus V. N.; Baddeley, Thomas C.; Wardell, James L.; Wardell, Solange M. S. V.

    2017-01-01

    The crystal structures of four 1-aryl-[1,2,4]triazolo[4,3-a]quinoxaline derivatives, 2, are reported: [aryl = 3-ClC6H4: 2a; 2-HOC6H4:2b;2,3-(HO)2C6H3: 2c; and 3,4-(MeO)2C6H3: 2d] The compounds, 2, were prepared by oxidation of substituted arenealdehyde quinoxalin-2-ylhydrazones, 1, using ferric chloride in alcohol. In each of the four compounds, the three ring -[1,2,4]triazolo[4,3-a]quinoxaline moiety is a near planar moiety, with all ring atoms within 0.1 Å of the best plane. There are large dihedral angles, 59 ± 7°, between the [1,2,4]triazolo[4,3-a]quinoxaline system and the phenyl ring. The ortho sited hydroxyl groups in 2c are jointly involved in a single Osbnd H⋯O intramolecular hydrogen bond and individually in Osbnd H⋯N intermolecular interactions, while the hydroxyl group in 2b is involved in an intermolecular Osbnd H⋯N hydrogen bond. These and weaker intermolecular interactions, including some of Csbnd H···Z (Z = O, N and or π) and π···π interactions generate the supramolecular arrangements in 2b and 2c. Intermolecular Csbnd H···Z (Z = O, N and or π) and π···π interactions are only present in 2a and 2d.

  5. Synthesis and fluorescence properties of 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazol derivatives and their terbium complexes.

    PubMed

    Zhang, Wu; Chai, Yuchao; Li, Kangyun; Chen, Yanwen; Yan, Dong; Guo, Dongcai

    2014-12-01

    Eight novel 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazol derivatives have been designed and synthesized, and their corresponding Tb(3+) complexes were also prepared successfully. The fluorescence properties and fluorescence quantum yields of the target complexes were investigated, the results showed that the ligands were an efficient sensitizer for Tb(3+) luminescence, and the target complexes exhibited characteristic fluorescence emissions of Tb(3+) ion. The fluorescence intensity of the complex substituted by chlorine was stronger than that of other complexes. The substituents' nature has a great effect upon the electrochemical properties of the target complexes. The results showed that the introduction of the electron-withdrawing groups tended to decrease the oxidation potential and highest occupied molecular orbital energy levels of the target Tb(3+) complexes; however, introduction of the electron-donating groups can increase the corresponding complexes' oxidation potential and highest occupied molecular orbital energy levels.

  6. Elastic Form Factors of 3,4He up to Large Q2

    SciTech Connect

    Kees De Jager

    2007-09-10

    Elastic electron scattering off $^3$He and $^4$He has recently been studied at forward and backward scattering angles in Hall A at JLab. The results will provide accurate data on the elastic form factors, charge and magnetic for $^3$He and charge only for $^4$He, up to squared momentum transfer $Q^2$-values of 3.2 GeV$^2$.

  7. Crystal structure of alluaudite-type NaMg3(HPO4)2(PO4)

    PubMed Central

    Ould Saleck, Ahmed; Assani, Abderrazzak; Saadi, Mohamed; Mercier, Cyrille; Follet, Claudine; El Ammari, Lahcen

    2015-01-01

    The title compound, sodium trimagnesium bis­(hydrogen phosphate) phosphate, was obtained under hydro­thermal conditions. In the crystal, two types of [MgO6] octa­hedra, one with point group symmetry 2, share edges to build chains extending parallel to [10-1]. These chains are linked together by two kinds of phosphate tetra­hedra, HPO4 and PO4, the latter with point group symmetry 2. The three-dimensional framework delimits two different types of channels extending along [001]. One channel hosts the Na+ cations (site symmetry 2) surrounded by eight O atoms, with Na—O bond lengths varying between 2.2974 (13) and 2.922 (2) Å. The OH group of the HPO4 tetra­hedron points into the other type of channel and exhibits a strong hydrogen bond to an O atom of the PO4 tetra­hedron on the opposite side. PMID:26279874

  8. A detailed study of antibacterial 3-acyltetramic acids and 3-acylpiperidine-2,4-diones.

    PubMed

    Jeong, Yong-Chul; Bikadi, Zsolt; Hazai, Eszter; Moloney, Mark G

    2014-08-01

    Inspired by the core fragment of antibacterial natural products such as streptolydigin, 3-acyltetramic acids and 3-acylpiperidine-2,4-diones have been synthesised from the core heterocycle by direct acylation with the substituted carboxylic acids using a strategy which permits ready access to a structurally diverse compound library. The antibacterial activity of these systems has been established against a panel of Gram-positive and Gram-negative bacteria, with activity mostly against the former, which in some cases is very potent. Data consistent with modes of action against undecaprenylpyrophosphate synthase (UPPS) and/or RNA polymerase (RNAP) for a small subset of the library has been obtained. The most active compounds have been shown to exhibit binding at known binding sites of streptolydigin and myxopyronin at UPPS and RNAP. These systems offer potential for their antibacterial activity, and further demonstrate the use of natural products as biologically validated starting points for drug discovery.

  9. Synthesis and biological activity of hydrazide hydrazones and their corresponding 3-acetyl-2,5-disubstituted-2,3-dihydro-1,3,4-oxadiazoles

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Various new 3-acetyl-2,5-disubstituted-2,3-dihydro-1,3,4-oxadiazoles (11-20) were prepared by the reaction of aryl substituted hydrazones of 4-fluorobenzoic acid hydrazide (1-10) with acetic anhydride. The structures of the newly synthesized compounds 11-20, were confirmed by UV, IR and 1H NMR spec...

  10. Diode-pumped Nd:YVO4 laser emitting at 1074 nm based on the 4 F 3/2-4 I 11/2 transition

    NASA Astrophysics Data System (ADS)

    Ma, Z. Y.; Li, C. L.; Liang, W.; Wang, J. G.

    2011-09-01

    We report a diode-pumped Nd:YVO4 laser emitting at 1074 nm, based on the 4 F 3/2-4 I 11/2 transition, generally used for a 1064 nm emission. A power of 323 mW at 1074 nm has been achieved in continuouswave (CW) operation with a fiber-coupled laser diode emitting 18.2 W at 808 nm. Intracavity second-harmonic generation in CW mode has also been demonstrated with a power of 18 mW at 537 nm by using a LiB3O5 (LBO) nonlinear crystal.

  11. Toxicity of 3,3',4,4'- and 2,2',5,5'-tetrabromobiphenyl: correlation of activity with aryl hydrocarbon hydroxylase induction and lack of protection by antioxidants.

    PubMed

    Robertson, L W; Andres, J L; Safe, S H; Lovering, S L

    1983-01-01

    3,3',4,4'-Tetrabromobiphenyl is a minor component of commercial polybrominated biphenyl (PBB) mixture fireMaster BP-6 and is a potent inducer of aryl hydrocarbon hydroxylase (AHH). A single ip dose of 3,3',4,4'-tetrabromobiphenyl (150 mumol/kg) caused significant reduction in the growth rate in the immature male Wistar rat, as well as pale enlarged livers and marked reduction in thymus size. Under light microscopy, hepatocytes were enlarged and vacuolated. The vacuoles, which were most prominent in the midzonal region of the lobule, corresponded to fat droplets in oil-red-O-stained sections. The thymus, especially the cortex, was markedly depleted of lymphocytes. Neither the reduced growth, altered organ weights nor the histopathology was reversed for the duration of the study by the coadministration of the antioxidants butylated hydroxy anisole (BHA), butylated hydroxy toluene (BHT), or vitamin E. Vitamin E did, however counter the negative effect of 3,3',4,4'-tetrabromobiphenyl on growth during the first 5 d of the study. 2,2',5,5'-Tetrabromobiphenyl, also a minor component of fireMaster BP-6, is a weak phenobarbital-type inducer of cytochrome P-450. When administered at the same dose, 2,2',5,5'-tetrabromobiphenyl did not elicit any observed toxic effects. These data confirm the correlation between AHH induction and toxicity for these PBBs and suggest that 3,3',4,4'-tetrabromobiphenyl may significantly contribute to the toxicity of fireMaster BP-6. Although there is evidence that polychlorinated biphenyls, and perhaps 2,3,7,8-tetrachlorodibenzo-p-dioxin, exert certain toxic effects via a lipid peroxidation mechanism, the toxic changes measured during this study were not reversed by the administration of the antioxidants.

  12. Outcomes of the 5-4-3-2-1 Go Childhood Obesity Community Trial

    ERIC Educational Resources Information Center

    Evans, W. Douglas; Christoffel, Katherine K.; Necheles, Jonathan; Becker, Adam B.; Snider, Jeremy

    2011-01-01

    Objectives: To determine effects of the "5-4-3-2-1 Go" community social marketing campaign on obesity risk factors. Methods: We randomly assigned 524 parents of 3- to 7-year-old children to receive "5-4-3-2-1 Go" counseling or not. We surveyed parents about "5-4-3-2-1 Go!" behaviors and perceptions of children's behaviors at baseline and one year…

  13. Hydrogen-bonded structures of the isomeric compounds of phthalazine with 3-chloro-2-nitrobenzoic acid, 4-chloro-2-nitrobenzoic acid and 4-chloro-3-nitrobenzoic acid.

    PubMed

    Gotoh, Kazuma; Ishida, Hiroyuki

    2011-11-01

    The structures of three isomeric compounds, C(7)H(4)ClNO(4)·C(8)H(6)N(2), of phthalazine with chloro- and nitro-substituted benzoic acid, namely, 3-chloro-2-nitrobenzoic acid-phthalazine (1/1), (I), 4-chloro-2-nitrobenzoic acid-phthalazine (1/1), (II), and 4-chloro-3-nitrobenzoic acid-phthalazine (1/1), (III), have been determined at 190 K. In the asymmetric unit of each compound, there are two crystallographically independent chloronitrobenzoic acid-phthalazine units, in each of which the two components are held together by a short hydrogen bond between an N atom of the base and a carboxyl O atom. In one hydrogen-bonded unit of (I) and in two units of (II), a weak C-H···O interaction is also observed between the two components. The N···O distances are 2.5715 (15) and 2.5397 (17) Å for (I), 2.5655 (13) and 2.6081 (13) Å for (II), and 2.613 (2) and 2.589 (2) Å for (III). In both hydrogen-bonded units of (I) and (II), the H atoms are each disordered over two positions with (N site):(O site) occupancies of 0.35 (3):0.65 (3) and 0.31 (3):0.69 (3) for (I), and 0.32 (3):0.68 (3) and 0.30 (3):0.70 (3) for (II). The H atoms in the hydrogen-bonded units of (III) are located at the O-atom sites.

  14. 3-Hydroxy-4-pyrones as Precursors of 4-Methoxy-3-oxidopyridinium Ylides. An Expeditious Entry to Highly Substituted 8-Azabicyclo[3.2.1]octanes.

    PubMed

    Rumbo, Antonio; Mouriño, Antonio; Castedo, Luis; Mascareñas, José L.

    1996-09-06

    3-Hydroxy-4-pyridones, which are easily prepared from commercially available 3-hydroxy-4-pyrones, can be readily transformed into 4-methoxy-3-oxidopyridinium ylides by treatment with methyl trifluoromethanesulfonate and subsequent deprotonation with a non-nucleophilic base. These ylides are capable of undergoing cycloaddition to several electron-deficient alkenes, thus allowing the synthesis of highly functionalized azabicyclo[3.2.1]octane moieties. The rich substitution patterns of these frameworks might allow their divergent conversion to a variety of natural and non-natural tropane alkaloids.

  15. Triangular oxalate clusters [W(3)(mu(3)-S)(mu(2)-S(2))(3)(C(2)O(4))(3)](2)(-) as building blocks for coordination polymers and nanosized complexes.

    PubMed

    Sokolov, Maxim N; Gushchin, Artem L; Kovalenko, Konstantin A; Peresypkina, Eugenia V; Virovets, Alexander V; Sanchiz, Joaquin; Fedin, Vladimir P

    2007-03-19

    The reaction of aqueous [W3S7(C2O4)3](2-) with Ln(3+) and Th(4+) in a 1:1 molar ratio leads to oxalate-bridged heteropolynuclear molecular complexes and coordination polymers. La(3+) and Ce(3+) give a layered structure with big (about 1.8 nm) honeycomb pores which are filled with water molecules and lanthanide ions, in {[Ln(H2O)6]3[W3S7(C2O4)3]4}Br x xH2O (Ia and Ib). The smaller Pr(3+), Nd(3+), Sm(3+), Eu(3+), and Gd(3+) ions give discrete nanomolecules [(W3S7(C2O4)3Ln(H2O)5)2(mu-C2O4)] (with a separation of about 3.2 nm between the most distant parts of the molecule), which are further united into zigzag chains by specific S2...Br- contacts to achieve the overall stoichiometry K[(W3S7(C2O4)3Ln(H2O)5)2(mu-C2O4)]Br.xH2O (IIa-IId). Th(4+) gives K2[(W3S7(C2O4)3)4Th2(OH)2(H2O)10] x 14.33H2O (III) with a nanosized discrete anion (with a separation of about 2.7 nm between the most distant parts of the molecule), in which two thorium atoms are bound via two hydroxide groups into the Th2(OH)2(6+) unit, and each Th is further coordinated by five water molecules and two monodentate [W3S7(C2O4)](2-) cluster ligands. All compounds were characterized by X-ray structure analysis and IR spectroscopy. Magnetic susceptibility measurements in the temperature range of 2-300 K show weak antiferromagnetic interactions between two lanthanides atoms for compounds IIa, IIb, and IId. The thermal decomposition of Ia, Ib, and IIb was studied by thermogravimetry.

  16. A computational study of simultaneous cation/anion interactions in model clusters containing all-cis 1,2,3-trifluorocyclopropane (F3C3H3) and all-cis 1,2,3,4-tetrafluorobutane (F4C4H4)

    NASA Astrophysics Data System (ADS)

    McDowell, Sean A. C.

    2016-11-01

    A computational study of two model clusters involving the all-cis 1,2,3-trifluorocyclopropane (F3C3H3) and the all-cis 1,2,3,4-tetrafluorocyclobutane (F4C4H4) molecules was undertaken. These clusters involve the simultaneous attachment of a cation (Li+/Na+) to the "negative" face of F3C3H3/F4C4H4 (via interaction with the Csbnd F bonds) and a model F- anion to the "positive" face of F3C3H3/F4C4H4 (via the adjacent Csbnd H bonds). The relative stabilities of the two model clusters was investigated and extended to the neutral M+sbnd F4C4H4sbnd X- (M = Li, Na, K; X = F, Cl, Br) clusters. The cation-anion electrostatic interaction is the main source of attraction in these highly polar moieties.

  17. Investigations on the 4-Quinolone-3-carboxylic Acid Motif. 7. Synthesis and Pharmacological Evaluation of 4-Quinolone-3-carboxamides and 4-Hydroxy-2-quinolone-3-carboxamides as High Affinity Cannabinoid Receptor 2 (CB2R) Ligands with Improved Aqueous Solubility.

    PubMed

    Mugnaini, Claudia; Brizzi, Antonella; Ligresti, Alessia; Allarà, Marco; Lamponi, Stefania; Vacondio, Federica; Silva, Claudia; Mor, Marco; Di Marzo, Vincenzo; Corelli, Federico

    2016-02-11

    4-Quinolone-3-carboxamide derivatives have long been recognized as potent and selective cannabinoid type-2 receptor (CB2R) ligands. With the aim to improve their physicochemical properties, basically aqueous solubility, two different approaches were followed, entailing the substitution of the alkyl chain with a basic replacement or scaffold modification to 4-hydroxy-2-quinolone structure. According to the first approach, compound 6d was obtained, showing slightly reduced receptor affinity (K(i) = 60 nM) compared to the lead compound 4 (0.8 nM) but greatly enhanced solubility (400-3400 times depending on the pH of the medium). On the other hand, shifting from 4-quinolone to 4-hydroxy-2-quinolone structure enabled the discovery of a novel class of CB2R ligands, such as 7b and 7c, characterized by K(i) < 1 nM and selectivity index [SI = K(i)(CB1R)/K(i)(CB2R)] > 1300. At pH 7.4, compound 7c resulted by 100-fold more soluble than 4.

  18. Enhanced visible-light photoactivity of g-C3N4 via Zn2SnO4 modification

    NASA Astrophysics Data System (ADS)

    Zhang, Lihong; Wang, Xiaoxing; Nong, Qingyan; Lin, Hongjun; Teng, Botao; Zhang, Yuting; Zhao, Leihong; Wu, Tinghua; He, Yiming

    2015-02-01

    The objective of this research was to prepare, characterize and evaluate the photocatalytic activity of Zn2SnO4/g-C3N4 composite in RhB degradation under visible light irradiation. The composite was synthesized by simple calcination of Zn2SnO4-melamine mixture, and was characterized by various techniques including Brunauer-Emmett-Teller method (BET), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (DRS), and photoluminescence spectroscopy (PL). Characterization results indicated that the decoration of Zn2SnO4 on g-C3N4 showed nearly no effect on its light absorption performance, but promoted the surface area of the composite, which benefited the adsorption of dyes and the subsequent photocatalytic process. However, more significant was the formation of hetero-junction structure between Zn2SnO4 and g-C3N4, which efficiently promoted the separation of electron-hole pairs and enhanced the photocatalytic performance of Zn2SnO4/g-C3N4. The optimal Zn2SnO4/g-C3N4 photocatalyst showed a degradation rate of 0.038 min-1, which was 3.2 times higher than that of g-C3N4. In addition, the Zn2SnO4/g-C3N4 composite shows high stability. rad O2- and h+ were the main reactive species.

  19. Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene from 3,5-dichloranisole

    DOEpatents

    Ott, Donald G.; Benziger, Theodore M.

    1990-01-01

    Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) from 3,5-dichloroanisole. Nitration of 3,5-dichloroanisole under relatively mild conditions gave 3,5-dichloro-2,4,6-trinitroanisole in high yield and purity. Ammonolysis of this latter compound gave the desired TATB. Another route to TATB was through the treatment of the 3,5-dichloro-2,4,6-trinitroanisole with thionyl chloride and dimethylformamide to yield 1,3,5-trichloro-2,4,6-trinitrobenzene. Ammonolysis of this product produced TATB.

  20. Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene from 3,5-dichloroanisole

    DOEpatents

    Ott, Donald G.; Benziger, Theodore M.

    1991-01-01

    Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) from 3,5-dichloroanisole. Nitration of 3,5-dichloroanisole under relatively mild conditions gave 3,5-dichloro-2,4,6-trinitroanisole in high yield and purity. Ammonolysis of this latter compound gave the desired TATB. Another route to TATB was through the treatment of the 3,5-dichloro-2,4,6-trinitroanisole with thionyl chloride and dimethylformamide to yield 1,3,5-trichloro-2,4,6-trinitrobenzene. Ammonolysis of this product produced TATB.

  1. Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene from 3,5-dichloroanisole

    DOEpatents

    Ott, D.G.; Benziger, T.M.

    1991-03-05

    Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) from 3,5-dichloroanisole is described. Nitration of 3,5-dichloroanisole under relatively mild conditions gave 3,5-dichloro-2,4,6-trinitroanisole in high yield and purity. Ammonolysis of this latter compound gave the desired TATB. Another route to TATB was through the treatment of the 3,5-dichloro-2,4,6-trinitroanisole with thionyl chloride and dimethylformamide to yield 1,3,5-trichloro-2,4,6-trinitrobenzene. Ammonolysis of this product produced TATB. 8 figures.

  2. Phosphate Ca1/4Sr1/4Zr2(PO4)3 of the NaZr2(PO4)3 structure type: Synthesis of a dense ceramic material and its radiation testing

    NASA Astrophysics Data System (ADS)

    Orlova, A. I.; Volgutov, V. Yu.; Mikhailov, D. A.; Bykov, D. M.; Skuratov, V. A.; Chuvil'deev, V. N.; Nokhrin, A. V.; Boldin, M. S.; Sakharov, N. V.

    2014-03-01

    The powder of phosphate Ca1/4Sr1/4Zr2(PO4)3 was synthesized by sol-gel processes in the presence of citric acid and ethylene glycol. Ceramic samples were prepared from this powder by Spark Plasma Sintering (SPS), their relative densities were found to be 99.5 ± 0.3% after the isothermal treatment at 860 °С for 3 min.

  3. Oct3/4 directly regulates expression of E2F3a in mouse embryonic stem cells

    SciTech Connect

    Kanai, Dai; Ueda, Atsushi; Akagi, Tadayuki; Yokota, Takashi; Koide, Hiroshi

    2015-04-10

    Embryonic stem (ES) cells, derived from the inner cell mass of blastocysts, have a characteristic cell cycle with truncated G1 and G2 phases. Recent findings that suppression of Oct3/4 expression results in a reduced proliferation rate of ES cells suggest the involvement of Oct3/4 in the regulation of ES cell growth, although the underlying molecular mechanism remains unclear. In the present study, we identified E2F3a as a direct target gene of Oct3/4 in ES cells. Oct3/4 directly bound to the promoter region of the E2F3a gene and positively regulated expression of E2F3a in mouse ES cells. Suppression of E2F3a activity by E2F6 overexpression led to the reduced proliferation in ES cells, which was relieved by co-expression of E2F3a. Furthermore, cell growth retardation caused by loss of Oct3/4 was rescued by E2F3a expression. These results suggest that Oct3/4 upregulates E2F3a expression to promote ES cell growth. - Highlights: • Oct3/4 positively regulates E2F3a expression in ES cells. • Oct3/4 binds to the promoter region of the E2F3a gene. • Overexpression of E2F6, an inhibitor of E2F3a, reduces ES cell growth. • E2F3a recovers growth retardation of ES cells caused by Oct3/4 reduction.

  4. 2-Methyl-sulfanyl-5,6-dihydro-2H-1,3-dithiolo[4,5-b][1,4]dioxin-2-ium tetra-fluoro-borate.

    PubMed

    Zhou, Guoquan; Chen, Xinzhi

    2012-04-01

    The title compound, C(6)H(7)O(2)S(3) (+)·BF(4) (-), consists of a planar 2-thioxo-1,3-dithiol-4,5-yl unit [maximum deviation from the ring plane = 0.020 (3) Å], with an ethyl-enedi-oxy group fused at the 4,5-positions; the ethyl-enedi-oxy C atoms are disordered over two positions with site-occupancy factors of 0.5. The 1,4-dioxine ring has a twist-chair conformation. Weak cation-anion S⋯F inter-actions [3.022 (4)-3.095 (4) Å] and an S⋯O [3.247 (4) Å] inter-action are present.

  5. Polymorphs of Li 3PO 4 and Li 2MSiO 4 (M = Mn, Co) . The role of pressure

    NASA Astrophysics Data System (ADS)

    Arroyo y de Dompablo, M. E.; Amador, U.; Gallardo-Amores, J. M.; Morán, E.; Ehrenberg, H.; Dupont, L.; Dominko, R.

    The behavior of Li 3PO 4 and Li 2MSiO 4 (M = Mn, Co) compounds under high pressure/high temperature is investigated. Pmn2 1-Li 3PO 4 remains stable up to the higher experimental limit of 80 kbar (900 °C). A sample of Li 2MnSiO 4 consisting of a mixture of Pn2 1 and Pmnb polymorphs converts upon high pressure/high temperature treatment into the Pmn2 1 polymorph; the latter being stable at 80 kbar and 900 °C. A sample of Li 2CoSiO 4- P2 1 /n transforms to the denser Pmn2 1 polymorph at 40 kbar/900 °C, but decomposes at higher pressure (60 kbar/900 °C). No evidence on any novel Li 2MSiO 4 polymorph is detected in any of the high-pressure products.

  6. 40 CFR 721.5252 - 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-, zinc salt.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...-methylenebis [3-hydroxy-, zinc salt. 721.5252 Section 721.5252 Protection of Environment ENVIRONMENTAL...′-methylenebis [3-hydroxy-, zinc salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-,...

  7. 40 CFR 721.5252 - 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-, zinc salt.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ...-methylenebis [3-hydroxy-, zinc salt. 721.5252 Section 721.5252 Protection of Environment ENVIRONMENTAL...′-methylenebis [3-hydroxy-, zinc salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-,...

  8. 40 CFR 721.5252 - 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-, zinc salt.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ...-methylenebis [3-hydroxy-, zinc salt. 721.5252 Section 721.5252 Protection of Environment ENVIRONMENTAL...′-methylenebis [3-hydroxy-, zinc salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-,...

  9. 40 CFR 721.5252 - 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-, zinc salt.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...-methylenebis [3-hydroxy-, zinc salt. 721.5252 Section 721.5252 Protection of Environment ENVIRONMENTAL...′-methylenebis [3-hydroxy-, zinc salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-,...

  10. 40 CFR 721.5252 - 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-, zinc salt.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ...-methylenebis [3-hydroxy-, zinc salt. 721.5252 Section 721.5252 Protection of Environment ENVIRONMENTAL...′-methylenebis [3-hydroxy-, zinc salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as 2-Naphthalenecarboxylic acid, 4,4′-methylenebis [3-hydroxy-,...

  11. Photoabsorption and photoionization cross sections of NH3, PH3, H2S, C2H2, and C2H4 in the VUV region

    NASA Technical Reports Server (NTRS)

    Xia, T. J.; Chien, T. S.; Wu, C. Y. Robert; Judge, D. L.

    1991-01-01

    Using synchrotron radiation as a continuum light source, the photoabsorption and photoionization cross sections of NH3, PH3, H2S, C2H2, and C2H4 have been measured from their respective ionization thresholds to 1060 A. The vibrational constants associated with the nu(2) totally symmetric, out-of-plane bending vibration of the ground electronic state of PH3(+) have been obtained. The cross sections and quantum yields for producing neutral products through photoexcitation of these molecules in the given spectral regions have also been determined. In the present work, autoionization processes were found to be less important than dissociation and predissociation processes in NH3, PH3, and C2H4. Several experimental techniques have been employed in order to examine the various possible systematic errors critically.

  12. (2R,3S,4R)-3,4-Isopropyl­idenedi­oxy-2-(phenyl­sulfonyl­meth­yl)pyrrolidin-1-ol

    PubMed Central

    Flores, Mari Fe; Garcia, Pilar; M. Garrido, Narciso; Sanz, Francisca; Diez, David

    2012-01-01

    The title compound, C14H19NO5S, was prepared by nucleophilic addition of the lithium derivative of methyl­phenyl­sulfone to (3S,4R)-3,4-isopropyl­idene­dioxy­pyrroline 1-oxide. There are four mol­ecules in the asymmetric unit. The crystal structure determination confirms the configuration of the chiral centres as 2R,3S,4R. In the crystal, pairs of O—H⋯N hydrogen bonds link the mol­ecules into dimers. PMID:22904989

  13. Hyperfine structures of the 2 (3)Sigma(g) (+), 3 (3)Sigma(g) (+), and 4 (3)Sigma(g) (+) states of Na(2).

    PubMed

    Liu, Yaoming; Li, Li; Lazarov, Guenadiy; Lazoudis, Angelos; Lyyra, A Marjatta; Field, Robert W

    2004-09-22

    The hyperfine structures of the 2 (3)Sigma(g) (+), 3 (3)Sigma(g) (+), and 4 (3)Sigma(g) (+) states of Na(2) have been resolved with sub-Doppler continuous wave perturbation facilitated optical-optical double resonance spectroscopy via A (1)Sigma(u) (+) approximately b (3)Pi(u) mixed intermediate levels. The hyperfine patterns of these three states are similar. The hyperfine splittings of the low rotational levels are all very close to the case b(betaS) limit. As the rotational quantum number increases, the hyperfine splittings become more complicated and the coupling cases become intermediate between cases b(betaS) and b(beta J) due to spin-rotation interaction. We present a detailed analysis of the hyperfine structures of these three (3)Sigma(g) (+) states, employing both case b(betaS) and b(beta J) coupling basis sets. The results show that the hyperfine splittings of the (3)Sigma(g) (+) states are mainly due to the Fermi-contact interaction. The Fermi contact constants for the two d sigma Rydberg states, the 2 (3)Sigma(g) (+) and 4 (3)Sigma(g) (+), are 245+/-5 MHz and 225+/-5 MHz, respectively, while the Fermi contact constant of the s sigma 3 (3)Sigma(g) (+) Rydberg state is 210+/-5 MHz. The diagonal spin-spin and spin-rotation constants, and nuclear spin-electronic spin dipolar interaction parameters of the 3 (3)Sigma(g) (+) and 4 (3)Sigma(g) (+) states are also obtained.

  14. High-resolution spectroscopy of Saturn at 3 microns: CH 4, CH 3D, C 2H 2, C 2H 6, PH 3, clouds, and haze

    NASA Astrophysics Data System (ADS)

    Kim, Joo Hyeon; Kim, Sang J.; Geballe, Thomas R.; Kim, Sungsoo S.; Brown, Linda R.

    2006-12-01

    We report observation and analysis of a high-resolution 2.87-3.54 μm spectrum of the southern temperate region of Saturn obtained with NIRSPEC at Keck II. The spectrum reveals absorption and emission lines of five molecular species as well as spectral features of haze particles. The ν+ν band of CH 3D is detected in absorption between 2.87 and 2.92 μm; and we derived from it a mixing ratio approximately consistent with the Infrared Space Observatory result. The ν band of C 2H 2 also is detected in absorption between 2.95 and 3.05 μm; analysis indicates a sudden drop in the C 2H 2 mixing ratio at 15 mbar (130 km above the 1 bar level), probably due to condensation in the low stratosphere. The presence of the ν+ν+ν band of C 2H 6 near 3.07 μm, first reported by Bjoraker et al. [Bjoraker, G.L., Larson, H.P., Fink, U., 1981. Astrophys. J. 248, 856-862], is confirmed, and a C 2H 6 condensation altitude of 10 mbar (140 km) in the low stratosphere is determined. We assign weak emission lines within the 3.3 μm band of CH 4 to the ν band of C 2H 6, and derive a mixing ratio of 9±4×10 for this species. Most of the C 2H 6 3.3 μm line emission arises in the altitude range 460-620 km (at ˜μbar pressure levels), much higher than the 160-370 km range where the 12 μm thermal molecular line emission of this species arises. At 2.87-2.90 μm the major absorber is tropospheric PH 3. The cloud level determined here and at 3.22-3.54 is 390-460 mbar (˜30 km), somewhat higher than found by Kim and Geballe [Kim, S.J., Geballe, T.R., 2005. Icarus 179, 449-458] from analysis of a low resolution spectrum. A broad absorption feature at 2.96 μm, which might be due to NH 3 ice particles in saturnian clouds, is also present. The effect of a haze layer at about 125 km (˜12 mbar level) on the 3.20-3.54 μm spectrum, which was not apparent in the low resolution spectrum, is clearly evident in the high resolution data, and the spectral properties of the haze particles suggest that

  15. Energetic Materials Based on 5,5'-Diamino-4,4'-dinitramino-3,3'-bi-1,2,4-triazole.

    PubMed

    Klapötke, Thomas M; Leroux, Marcel; Schmid, Philipp C; Stierstorfer, Jörg

    2016-03-18

    A simple and straightforward synthesis of 5,5'-diamino-4,4'-dinitramino-3,3'-bi-1,2,4-triazole by the selective nitration of 4,4',5,5'-tetraamino-3,3'-bi-1,2,4-triazole is presented. The interaction of the amino and nitramino groups improves the energetic properties of this functionalized bitriazole. For a deeper investigation of these properties, various nitrogen-rich derivatives were synthesized. The new compounds were investigated and characterized by spectroscopy ((1)H and (13)C NMR, IR, Raman), elemental analysis, mass spectrometry, differential thermal analysis (DTA), X-ray analysis, and impact and friction sensitivities (IS, FS). X-ray analyses were performed and deliver insight into structural characteristics with which the stability of the compounds can be explained. The standard enthalpies of formation were calculated for all compounds at the CBS-4M level of theory, revealing highly positive heats of formation. The energetic performance of the new molecules was predicted with the EXPLO5 V6.02 computer. A small-scale shock reactivity test (SSRT) and a toxicity test gave a first impression of the performance and toxicity of selective compounds.

  16. X-ray studies of 2-amino-5-oxo-4-propyl-4,5-dihydropyrano[3,2- c]chromene-3-carbonitrile

    NASA Astrophysics Data System (ADS)

    Sharma, S.; Banerjee, B.; Brahmachari, G.; Kant, R.; Gupta, V. K.

    2015-11-01

    The carbonitrile compound, 2-amino-5-oxo-4-propyl-4,5-dihydropyrano[3,2- c]chromene-3-carbonitrile was synthesized, in 83% yield, by one-pot multicomponent reaction of butyraldehyde, malononitrile and 4-hydroxycoumarin using 10 mol% urea as an organo-catalyst at room temperature, and its crystal structure was determined by X-ray diffraction technique. The crystals are triclinic, a = 7.7379(5), b = 8.7520(6), c = 11.6589(5) Å, α = 96.668(4)°, β = 100.033(4)°, γ = 112.547(6)°, Z = 2, sp. gr. P. Both pyran rings in the molecule adopt a boat conformation. The crystal structure is stabilized by N-H···O and N-H···N hydrogen bonds.

  17. Luminescence of Eu and Ce in K3Ca2(SO4)3F fluoride material.

    PubMed

    Poddar, Anuradha; Gedam, S C; Dhoble, S J

    2015-09-01

    A new halophosphor K3Ca2(SO4)3F activated by Eu or Ce and K3Ca2(SO4)3F:Ce,Eu co-doped halosulfate phosphor has been synthesized by the co-precipitation method and characterized for its photoluminescence (PL). The PL emission spectra of the K3Ca2(SO4)3F:Ce phosphor show emission at 334 nm when excited at 278 nm due to 5d → 4f transition of Ce(3+) ions. In the K3Ca2(SO4)3F:Eu lattice, Eu(2+) (440 nm) as well as Eu(3+) (596 nm and 615 nm) emissions have been observed showing (5) D0 →(7) F1 and (5) D0 →(7) F2 transition of the Eu(3+) ion, which is in the blue and red region of the visible spectrum respectively. The trivalent europium ion is very useful for studying the nature of metal coordination in various systems owing to its non-degenerate emitting (5) D0 state. K3Ca2(SO4)3F:Ce,Eu is suitable for Ce(3+) → Eu(2+) → Eu(3+) energy transfer in which Ce(3+) and Eu(2+) play the role of sensitizers and Eu(2+) and Eu(3+) act as the activators. The observations presented in this paper are relevant for lamp phosphors.

  18. Ferroelastic phase transitions by 14N NMR spectra in [N(CH3)4]2CoCl4 and [N(CH3)4]2ZnCl4 single crystals

    NASA Astrophysics Data System (ADS)

    Lim, Ae Ran

    2016-09-01

    Changes in the structural geometry of [N(CH3)4]2BCl4 (B=Co and Zn) crystals near the phase transition temperatures were studied by analyzing the 14N nuclear magnetic resonance (NMR) spectra. Two physically inequivalent a-N(1)(CH3)4 and b-N(2)(CH3)4 groups were observed in these spectra. Abrupt changes in the resonance frequency and splitting of 14N NMR signals near the phase transition temperatures were attributed to structural phase transitions, and the primary mechanism of these phase transitions exhibited ferroelastic characteristics. In addition, ferroelasticity of [N(CH3)4]2BCl4 was identified at low temperatures using optical polarizing microscopy.

  19. Li3Al(MoO2)2O2(AsO4)2

    PubMed Central

    Hajji, Mounir; Zid, Mohamed Faouzi; Driss, Ahmed

    2009-01-01

    Single crystals of trilithium(I) aluminium(III) bis­[dioxidomolybdenum(VI)] dioxide bis­[arsenate(V)], Li3AlMo2As2O14, have been prepared by solid-state reaction at 788 K. The structure consists of AsO4 tetra­hedra, AlO6 octa­hedra and Mo2O10 groups sharing corners to form a three-dimensional framework containing channels running respectively along the [100] and [010] directions, where the Li+ ions are located. This structure is compared with compounds having (MX 2O12)n chains (M = Mo, Al and X = P, As) and others containing M 2O10 (M = Mo, Fe) dimers. PMID:21582037

  20. Phosphoinnelite, Ba4Na3Ti3Si4O14(PO4,SO4)2(O,F)3, a new mineral species from peralkaline pegmatite of the Kovdor pluton, Kola Peninsula

    NASA Astrophysics Data System (ADS)

    Pekov, I. V.; Chukanov, N. V.; Kulikova, I. M.; Belakovsky, D. I.

    2007-12-01

    Phosphoinnelite, an analogue of innelite with P > S, has been found in a peralkaline pegmatite vein crosscutting calcite carbonatite at the phlogopite deposit, Kovdor pluton, Kola Peninsula. Cancrinite (partly replaced with thomsonite-Ca), orthoclase, aegirine-augite, pectolite, magnesioarfvedsonite, golyshevite, and fluorapatite are associated minerals. Phosphoinnelite occurs as lath-shaped crystals up to 0.2 × 1 × 6 mm in size, which are combined typically in bunch-, sheaf-, and rosettelike segregations. The color is yellow-brown, with vitreous luster on crystal faces and greasy luster on broken surfaces. The mineral is transparent. The streak is pale yellowish. Phosphoinnelite is brittle, with perfect cleavage parallel to the {010} and good cleavage parallel to the {100}; the fracture is stepped. The Mohs hardness is 4.5 to 5. Density is 3.82 g/cm3 (meas.) and 3.92 g/cm3 (calc.). Phosphoinnelite is biaxial (+), α = 1.730, β = 1.745, and γ = 1.764, 2V (meas.) is close to 90°. Optical orientation is Z^c ˜ 5°. Chemical composition determined by electron microprobe is as follows (wt %): 6.06 Na2O, 0.04 K2O, 0.15 CaO, 0.99 SrO, 41.60 BaO, 0.64 MgO, 1.07 MnO, 1.55 Fe2O3, 0.27 Al2O3, 17.83 SiO2, 16.88 TiO2, 0.74 Nb2O5, 5.93 P2O5, 5.29 SO3, 0.14 F, -O=F2 = -0.06, total is 99.12. The empirical formula calculated on the basis of (Si,Al)4O14 is (Ba3.59Sr0.13K0.01)Σ3.73(Na2.59Mg0.21Ca0.04)Σ3.04(Ti2.80Fe{0.26/3+}Nb0.07)Σ3.13[(Si3.93Al0.07)Σ4O14(P1.11S0.87)Σ1.98O7.96](O2.975F0.10)Σ3.075. The simplified formula is Ba4Na3Ti3Si4O14(PO4,SO4)2(O,F)3. The mineral is triclinic, space group P overline 1 or P1. The unit cell dimensions are a = 5.38, b = 7.10, c = 14.76 Å; α = 99.00°, β = 94.94°, γ = 90.14°; and V = 555 Å3, Z = 1. The strongest lines of the X-ray powder pattern [ d, Å in ( I)( hkl)] are: 14.5(100)(001), 3.455(40)(103), 3.382(35)(0overline 2 2), 2.921(35)(005), 2.810(40)(1overline 1 4), 2.683(90)(200, overline 2 01), 2.133(80)(overline 2 overline

  1. Synthesis and Anticonvulsant Activity Evaluation of 3-alkoxy-4-(4-(hexyloxy/heptyloxy)phenyl)-4H-1,2,4 -triazole

    PubMed Central

    Fang, Ying-Quan; Sun, Chun-Ling; Liu, Da-Chuan; Wang, Shi-Ben; Quan, Zhe-San

    2015-01-01

    A series of 3-alkoxy-4-(4-(hexyloxy/heptyloxy) phenyl)-4H-1,2,4-triazole was synthesized. The anticonvulsant effect and neurotoxicity of the compounds were calculated with maximal electroshock (MES) test and rotarod tests with intraperitoneally injected mice. Among the synthesized compounds, compound 3-heptyloxy-4-(4-(hexyloxy) phenyl)-4H-1,2,4-triazole (5f) was the most active one and also had the lowest toxicity. In the anti-MES potency test, it showed median effective dose (ED50) of 37.3 mg/Kg, median toxicity dose (TD50) of 422.5 mg/Kg, and the protective index (PI) of 11.3 which is much greater than the reference drug carbamazepine with PI value of 6.4. As well as demonstrating the anti-MES efficacy of compound 5f, its potency against seizures induced by pentylenetetrazole, 3-mercaptopropionic acid, and bicuculline were also established, with the results suggesting that GABA-mediated mechanisms might be involved in its anticonvulsant activity, such as enhancing of GABAergic neurotransmission or activity, activate GAD or inhibit GABA-T, and GABAA-mediated mechanisms. PMID:25561914

  2. Reactivity study of 1H-thieno[3,2-d][1,3]oxazine-2,4-dione toward the synthesis of bicyclic 3,4-dihydro-1H-thieno[3,2-e][1,4]diazepine-2,5-dione analogues.

    PubMed

    Brouillette, Yann; Lisowski, Vincent; Fulcrand, Pierre; Martinez, Jean

    2007-03-30

    A series of 10 optically pure 3,4-dihydro-1H-thieno[3,2-e][1,4]diazepine-2,5-dione derivatives has been synthesized in 41-75% yields on treatment of 1H-thieno[3,2-d][1,3]oxazine-2,4-dione with different natural alpha-amino acids.

  3. Synthesis and antimicrobial activities of some novel 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles and 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazines carrying thioalkyl and sulphonyl phenoxy moieties.

    PubMed

    Karabasanagouda, T; Adhikari, Airody Vasudeva; Shetty, N Suchetha

    2007-04-01

    Thirty one new 6-aryl-3-{(4-substituted phenoxy) methyl}-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles (6a-s) and 6-aryl-3-[(4-substituted phenoxy methyl]-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazines (7a-l) have been synthesized from 4-thioalkyl phenols (1a-b) through a multi-step reaction sequence. Compounds 1a-b reacted with ethyl chloroacetate in presence of acetone and potassium carbonate to give ethyl [4-(thioalkyl) phenoxy] acetates (2a-b). Further, 2a was oxidized to [4-(methyl sulphonyl) phenoxy] acetate (2c) using hydrogen peroxide in acetic acid. Reactions of (2a-c) with hydrazine hydrate in alcoholic medium furnished 2-[4-thiosubstituted phenoxy] acetohydrazides (3a-b) and 2-[4-methyl sulphonyl phenoxy] acetohydrazide (3c) which on treatment with carbon disulphide and methanolic potassium hydroxide yielded corresponding potassium dithiocarbazates (4a-c). They were then converted to 4-amino-5-[(4-thioalkyl phenoxy) methyl]-4H-1,2,4-triazole-3-thiols (5a-b) and 4-amino-5-[(4-methyl sulphonyl phenoxy) methyl]-4H-1,2,4-triazole-3-thiol (5c) by refluxing them with aqueous hydrazine hydrate. The title compounds 6a-s were prepared by condensing 5a-c with various aromatic carboxylic acids in presence of phosphorus oxychloride. The intermediates 5a-c, on condensation with various substituted phenacyl bromides afforded a series of title compounds (7a-l). The structures of new compounds 2a-7l were established on the basis of their elemental analysis, IR, (1)H NMR, (13)C NMR and mass spectral data. All the title compounds were subjected to in vitro antibacterial testing against four pathogenic strains and antifungal screening against three fungi. Preliminary results indicate that some of them exhibited promising activities and they deserve more consideration as potential antimicrobials.

  4. Synthesis, characterization, and crystal structure of 2-amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[3,2-c] pyran-3-carbonitrile

    SciTech Connect

    Sharma, S.; Banerjee, B.; Brahmachari, G.; Kant, Rajni; Gupta, V. K.

    2015-12-15

    2-Amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[3,2-c] pyran-3-carbonitrile, C{sub 16}H{sub 12}N{sub 2}O{sub 3} is synthesized via one-pot multi-component reaction at room temperature using commercially available urea as inexpensive and environmentally benign organo-catalyst. Its structure is determined by single-crystal X-ray diffraction technique The crystals are monoclinic, a = 10.7357(12), b = 8.7774(8), c = 15.0759(16) Å, β = 103.575(11)°, Z = 4, sp. gr. P2{sub 1}/n, R = 0.0551 for 1696 observed reflections. The crystal structure is stabilized by N–H···N, C–H···O, and C–H···π interactions.

  5. Removal of nitrate and phosphate using chitosan/Al2O3/Fe3O4 composite nanofibrous adsorbent: Comparison with chitosan/Al2O3/Fe3O4 beads.

    PubMed

    Bozorgpour, Farahnaz; Ramandi, Hossein Fasih; Jafari, Pooya; Samadi, Saman; Yazd, Shabnam Sharif; Aliabadi, Majid

    2016-12-01

    In the present study the chitosan/Al2O3/Fe3O4 composite nanofibrous adsorbent was prepared by electrospinning process and its application for the removal of nitrate and phosphate were compared with chitosan/Al2O3/Fe3O4 composite bead adsorbent. The influence of Al2O3/Fe3O4 composite content, pH, contact time, nitrate and phosphate initial concentrations and temperature on the nitrate and phosphate sorption using synthesized bead and nanofibrous adsorbents was investigated in a single system. The reusability of chitosan/Al2O3/Fe3O4 composite beads and nanofibers after five sorption-desorption cycles were carried out. The Box-Behnken design was used to investigate the interaction effects of adsorbent dosage, nitrate and phosphate initial concentrations on the nitrate and phosphate removal efficiency. The pseudo-second-order kinetic model and known Freundlich and Langmuir isotherm models were used to describe the kinetic and equilibrium data of nitrate and phosphate sorption using chitosan/Al2O3/Fe3O4 composite beads and nanofibers. The influence of other anions including chloride, fluoride and sulphate on the sorption efficiency of nitrate and phosphate was examined. The obtained results revealed the higher potential of chitosan/Al2O3/Fe3O4 composite nanofibers for nitrate and phosphate compared with chitosan/Al2O3/Fe3O4 composite beads.

  6. Zinclipscombite, ZnFe{2/3+}(PO4)2(OH)2, a new mineral species

    NASA Astrophysics Data System (ADS)

    Chukanov, N. V.; Pekov, I. V.; Möckel, S.; Zadov, A. E.; Dubinchuk, V. T.

    2007-12-01

    Zinclipscombite, a new mineral species, has been found together with apophyllite, quartz, barite, jarosite, plumbojarosite, turquoise, and calcite at the Silver Coin mine, Edna Mountains, Valmy, Humboldt County, Nevada, United States. The new mineral forms spheroidal, fibrous segregations; the thickness of the fibers, which extend along the c axis, reaches 20 μm, and the diameter of spherulites is up to 2.5 mm. The color is dark green to brown with a light green to beige streak and a vitreous luster. The mineral is translucent. The Mohs hardness is 5. Zinclipscombite is brittle; cleavage is not observed; fracture is uneven. The density is 3.65(4) g/cm3 measured by hydrostatic weighing and 3.727 g/cm3 calculated from X-ray powder data. The frequencies of absorption bands in the infrared spectrum of zinclipscombite are (cm-1; the frequencies of the strongest bands are underlined; sh, shoulder; w, weak band) 3535, 3330sh, 3260, 1625w, 1530w, 1068, 1047, 1022, 970sh, 768w, 684w, 609, 502, and 460. The Mössbauer spectrum of zinclipscombite contains only a doublet corresponding to Fe3+ with sixfold coordination and a quadrupole splitting of 0.562 mm/s; Fe2+ is absent. The mineral is optically uniaxial and positive, ω = 1.755(5), ɛ = 1.795(5). Zinclipscombite is pleochroic, from bright green to blue-green on X and light greenish brown on Z ( X > Z). Chemical composition (electron microprobe, average of five point analyses, wt %): CaO 0.30, ZnO 15.90, Al2O3 4.77, Fe2O3 35.14, P2O5 33.86, As2O5 4.05, H2O (determined by the Penfield method) 4.94, total 98.96. The empirical formula calculated on the basis of (PO4,AsO4)2 is (Zn0.76Ca0.02)Σ0.78(Fe{1.72/3+} Al0.36)Σ2.08[(PO4)1.86(AsO4)0.14]Σ2.00(OH)1. 80 · 0.17H2O. The simplified formula is ZnFe{2/3+} (PO4)2(OH)2. Zinclipscombite is tetragonal, space group P43212 or P41212; a = 7.242(2) Å, c = 13.125(5) Å, V = 688.4(5) Å3, Z = 4. The strongest reflections in the X-ray powder diffraction pattern ( d, ( I, %) (( hkl

  7. (3,3-Difluoro-pyrrolidin-1-yl)-[(2S,4S)-(4-(4-pyrimidin-2-yl-piperazin-1-yl)-pyrrolidin-2-yl]-methanone: A potent, selective, orally active dipeptidyl peptidase IV inhibitor

    SciTech Connect

    Ammirati, Mark J.; Andrews, Kim M.; Boyer, David D.; Brodeur, Anne M.; Danley, Dennis E.; Doran, Shawn D.; Hulin, Bernard; Liu, Shenping; McPherson, R. Kirk; Orena, Stephen J.; Parker, Janice C.; Polivkova, Jana; Qiu, Xiayang; Soglia, Carolyn B.; Treadway, Judith L.; VanVolkenburg, Maria A.; Wilder, Donald C.; Piotrowski, David W.; Pfizer

    2010-10-01

    A series of 4-substituted proline amides was synthesized and evaluated as inhibitors of dipeptidyl pepdidase IV for the treatment of type 2 diabetes. (3,3-Difluoro-pyrrolidin-1-yl)-[(2S,4S)-(4-(4-pyrimidin-2-yl-piperazin-1-yl)-pyrrolidin-2-yl]-methanone (5) emerged as a potent (IC{sub 50} = 13 nM) and selective compound, with high oral bioavailability in preclinical species and low plasma protein binding. Compound 5, PF-00734200, was selected for development as a potential new treatment for type 2 diabetes.

  8. Quantum chemical study of ternary mixtures of: HNO3:H2SO4:H2O

    NASA Astrophysics Data System (ADS)

    Verdes, M. A.; Gómez, P. C.; Gálvez, O.

    2009-04-01

    Water, nitric acid and sulfuric acid are important atmospheric species as individual species and as hydrogen-bonded aggregates involved in many physical-chemical processes both superficial and bulk. The importance of heterogeneous chemical reactions taking place on ice surfaces, either solid water or solid water plus nitric or sulfuric acid, is well established now in relation to the ozone-depleting mechanisms. Also the importance of liquid droplets formed by HNO3.H2SO4.H2O as components of PSC was soon recognized [1-3]. Finally the physical properties of finely divided aqueous systems is an interesting and active field of research in which theoretical information on the microphysical domain systems may help to understand and rationalize the wealth of experimental information. This can also be the initial step in the study of more complex mixtures with higher amounts of water or variable proportions of their constituents. This kind of calculations have been successfully performed in the past[4]. We present here our results on the structure and spectroscopic and thermodynamic properties of the energy-lowest lying structures among those thermodynamically stable formed by linking the acids plus water. The calculations have been carried out by means of DFT methods (in particular the successful B3LYP) using different basis sets that contain appropriate sets of polarization and diffuse functions up to quadruple-Z quality (Dunninǵs aug-cc-pVQZ). Careful assessment of the dependability of the methodology used has been carried out. This work has been supported by the Spanish Ministry of Education, Projects FIS2007-61686 and CTQ2008-02578/BQU References: [1] Carslaw, K. S. et al.: Geophys. Res. Lett. 21, 2479-2482, 1994 [2] Drdla, K. Et al. :Geophys. Res. Lett. 21, 2473-2478, 1994 [3] Tabazadeh, A. et al.: Geophys. Res. Lett 21, 1619-1622, 1994 [4] Escribano, R et al.: J. J. Chem. Phys A 2003, 107, 652.

  9. Interleukin 2 promotes growth and cytolytic activity in human T3+4-8- thymocytes.

    PubMed Central

    de la Hera, A; Toribio, M L; Marquez, C; Martinez, C

    1985-01-01

    Human thymocytes bearing T3 but neither T4 nor T8 antigens (T3+4-8- cells) were obtained after negative selection of thymocytes, either fresh or cultured in medium containing recombinant interleukin 2 (IL-2), by treatment with Na1/34, OKT4A and B9.4 monoclonal antibodies (which recognize T6, T4, and T8 antigens, respectively) and complement. Quantitative flow cytometry showed a 98% pure population of T3+4-8- lymphocytes, which included proliferating cells. The growth and maturation requirements of these thymocytes were characterized and related to the T3-receptor complex and IL-2 pathways, thought to be used by mature lymphocytes. The results show that addition of recombinant IL-2 promotes, in a dose-dependent way, proliferation and acquisition of effector functions by cultured T3+4-8- thymocytes, the growth being inhibitable by monoclonal antibody 33B73 (anti-Tac). Furthermore, cytolytic activity of T3+4-8- cells induced by recombinant IL-2 is specifically blocked by monoclonal antibody OKT3, showing that it operates via the T3-receptor complex and does not require either T4 or T8 molecules. The finding of in vitro responsiveness to recombinant IL-2 in T3+4-8- thymocytes suggests a role of IL-2 in the growth and maturation of cells committed to the T-cell lineage, during intrathymic differentiation, prior to expression of T4 and T8 molecules. PMID:3929254

  10. The crystal chemistry of Ca(10-y)(SiO4)3(SO4)3Cl(2-x-2y)F(x) ellestadite.

    PubMed

    Fang, Yanan; Ritter, Clemens; White, Tim

    2011-12-19

    Fluor-chlorellestadite solid solutions Ca(10)(SiO(4))(3)(SO(4))(3)Cl(2-x)F(x), serving as prototype crystalline matrices for the fixation of hazardous fly ash, were synthesized and characterized by powder X-ray and neutron diffraction (PXRD and PND), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FTIR). The lattice parameters of the ellestadites vary linearly with composition and show the expected shrinkage of unit cell volume as fluorine (IR = 1.33 Å) displaces chlorine (IR = 1.81 Å). FTIR spectra indicate little or no OH(-) in the solid solutions. All compositions conform to P6(3)/m symmetry where F(-) is located at the 2a (0, 0, (1)/(4)) position, while Cl(-) is displaced out of the 6h Ca(2) triangle plane and occupies 4e (0, 0, z) split positions with z ranging from 0.336(3) to 0.4315(3). Si/S randomly occupy the 6h tetrahedral site. Ellestadites rich in Cl (x ≤ 1.2) show an overall deficiency in halogens (<2 atom per formula unit), particularly Cl as a result of CaCl(2) volatilization, with charge balance achieved by the creation of Ca vacancies (Ca(2+) + 2Cl(-) →□(Ca) + 2□(Cl)) leading to the formula Ca(10-y)(SiO(4))(3)(SO(4))(3)Cl(2-x-2y)F(x). For F-rich compositions the vacancies are found at Ca(2), while for Cl-rich ellestadites, vacancies are at Ca(1). It is likely the loss of CaCl(2) which leads tunnel anion vacancies promotes intertunnel positional disorder, preventing the formation of a P2(1)/b monoclinic dimorph, analogous to that reported for Ca(10)(PO(4))(6)Cl(2). Trends in structure with composition were analyzed using crystal-chemical parameters, whose systematic variations served to validate the quality of the Rietveld refinements.

  11. Yb3+-doped KLu(WO4)2, Nb:RbTiOPO4 and KGd(PO3)4 crystals. Growth, characterization and laser operation

    NASA Astrophysics Data System (ADS)

    Pujol, M. C.; Mateos, X.; Carvajal, J. J.; Solé, R.; Massons, J.; Aguiló, M.; Díaz, F.

    2017-01-01

    Macrodefect-free samples of Yb3+:KLu(WO4)2, Yb3+:Nb:RbTiOPO4 and Yb3+:KGd(PO3)4 laser crystals were grown using the Top Seeded Solution Growth - Slow Cooling technique. Structural and morphological studies related with the three materials were carried out and discussed. The dispersion of the refractive indices was measured and Sellmeier equations were constructed which are valid in the UV-Vis-IR range. The Stark splitting of the two electronic states of trivalent ytterbium was determined and the CW laser generation was demonstrated in these hosts. This paper shows a review of the main results achieved in FiCMA-FiCNA-URV laboratories in relation with these laser materials in the last years.

  12. Reaction of 1Н,2Н,3Н,4Н-pyrido[4,3-d]pyrimidinium bromide derivatives with molecular iodine: Comparative structure and spectroscopic analysis

    NASA Astrophysics Data System (ADS)

    Chernov'yants, Margarita S.; Burykin, Igor V.; Kostrub, Vladimir V.; Tsupak, Evgeny B.; Starikova, Zoya A.; Kirsanova, Julia A.

    2012-02-01

    New salts C27H22N3O2BrI2 (1) and C27H19N3O2Br4I2·2CHCl3·2H2O (2) were synthesized by the iodination of derivatives of 1,3-dimethyl-2,4-dioxo-5,6,7-R-1Н,2Н,3Н,4Н-pyrido[4,3-d]pyrimidinium bromide (R = phenyl (1a), p-bromphenyl (2a)) with an equimolar amount of iodine. The positive values of enthalpy (ΔH) and entropy (ΔS) indicate that the complexation of organic bromide and iodine molecule in chloroform solution is mainly entropically driven. The molecular and crystal structures (1) and (2) are studied by X-ray diffraction analysis. The structure of diiodinebromide 1 is composed of separate almost liner BrI2- and 1,3-dimethyl-2,4-dioxo-5,6,7-thriphenyl-1Н,2Н,3Н,4Н-pyrido[4,3-d]pyrimidinium cation. The crystal structure 2 is built up of alternate layers of (CHNOBr3+)(I3-) (A) and (Br2I-)(СHСl3) (B), connected to each other by hydrogen bonds Br(BrI)⋯H(CHNOBr3+). The formation of the ions I3- and Br2I- occurs via the disproportionation of I2Br- under the action of solvent on C27H19N3O2Br4I2·2CHCl3·2H2O (2) crystallization.

  13. 40 CFR 721.5262 - 2,7-Naphthalenedisulfonic acid, 5-[[4-chloro-6-[substituted] amino]-1,3,5-triazin-2-yl]amino]-4...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ...,7-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3- -, trisodium salt...-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3- -, trisodium salt (PMN P-00-0803) is...-naphthalenedisulfonic acid, 5- ethyl]amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3- -, sodium salt (1:3) (PMN......

  14. A novel monoterpene-stilbene adduct with a 4,4-dimethyl-2,3-diphenylchromane skeleton from Artocarpus xanthocarpus.

    PubMed

    Ko, Horng-Huey; Jin, Yu-Jing; Lu, Tzy-Ming; Chen, Ih-Sheng

    2013-07-01

    Artoxanthochromane (1), a DielsAlder-type conjugation product of 4-isopropenylresorcinol and oxyresveratrol, was isolated from the heartwood of Artocarpus xanthocarpus and characterized. The structure of 1 was elucidated as 2-(2,4-dihydroxyphenyl)-3-(3,5-dihydroxyphenyl)-7-hydroxy-4,4-dimethylchromane by 1D- and 2D-NMR spectroscopy, and other spectral evidences. A plausible metabolic mechanism was proposed to illustrate the biosynthetic pathway of artoxanthochromane. This compound exhibited mild mushroom tyrosinase inhibitory, and weak free radical-scavenging activities on ABTS(+.) and superoxide anion (O$\\rm{{_{2}^{-{^\\cdot} }}}$) free radicals.

  15. Synthesis of 5-alkoxythieno[2,3-e][1,2,4]triazolo[4,3-c]pyrimidine derivatives and evaluation of their anticonvulsant activities.

    PubMed

    Wang, Shi-Ben; Piao, Guang-Chun; Zhang, Hong-Jian; Quan, Zhe-Shan

    2015-04-15

    This work concerns the design and synthesis of novel, substituted 5-alkoxythieno[2,3-e][1,2,4]triazolo[4,3-c]pyrimidine derivatives 5a-p prepared from 3-amino-2-thiophenecarboxylic acid methyl ester. The final compounds were screened for their in vivo anticonvulsant activity using maximal electroshock (MES) and subcutaneous pentylenetetrazole (scPTZ) tests. Neurotoxicity (NT) was tested using a rotarod test. The structure-anticonvulsant activity relationship analysis revealed that the most effective structural motif involves a substituted phenol, especially when substituted with a single chlorine, fluorine or trifluoromethyl group (at the meta-position), or two chlorine atoms. These molecules possessed high activity according to the MES and scPTZ models. Quantitative assessment of the compounds after intraperitoneal administration in mice showed that the most active compound was 5-[3-(trifluoromethyl)phenoxy]thieno[2,3-e] [1,2,4]triazolo[4,3-c]pyrimidine (5o) with ED50 values of 11.5 mg/kg (MES) and 58.9 mg/kg (scPTZ). Furthermore, compound 5o was more effective in the MES and scPTZ tests than the well-known anticonvulsant drugs carbamazepine and ethosuximide.

  16. Metal complexes with some 3-aryl-1,2,4-oxadiazoles

    NASA Astrophysics Data System (ADS)

    Massacesi, Marcella; Devoto, Gerolamo; Gelli, Gioanna

    1985-01-01

    Complexes of empirical formula M(L) 2X 2 were synthesized and characterized, where L = 5-methyl-3-(2,4,6-trimethoxiphenyl)-1,2,4-oxadiazole (topho), M = Zn(II), Cu(II), Co(II), Pd(II), Pt(II), X = Cl, M = Pd(II), Pt(II), X = Br, M = Zn(II), X = I; L = 5-methy]-3-(3,5-dichloro,2,4,6-trimethyl-phenyl)-1,2,4-oxadiazole (ctpho), M = Cu(II), Co(II), X = Cl; L = 5-methyl-3-(2,4,6-trimethylphenyl)-1,2,4-oxadiazole (tpho), M = Cu(II), X = Cl. Magnetic, spectral, conductivity and elemental analysis data indicate that the ligands always act as monodentate, N-bonded. The Pd(II) and Pt(II) complexes are square planar and all the other derivatives are tetrahedral.

  17. Determination of 2-isovaleryl-1,3-indandione with 2, 4-dinitro-phenylhydrazine

    USGS Publications Warehouse

    Menzie, C.M.; Adomaitis, V.A.; Reichel, W.L.

    1962-01-01

    At present, three 2-alkyl-1,3-indandiones (PMP, pival, and diphacinon) are widely used as rodenticides. Because analytical procedures now in use are empirical and do not furnish adequate or positive means for distinguishing among these closely related compounds, studies were undertaken to develop a sensitive and specific method for the determination of PMP. The relation between KCN and the 2,4-dinitrophenylhydrazone of PMP was investigated and shown to be sensitive and specific. A deeply colored solution is produced with an absorption maximum at 540 mu. This solution obeys Beer?s law over a wide range. The molar absorptivity for the developed color was calculated to be 3.0 X 104. This reaction can be used also as a spot test to detect as little as 1 ug. of PMP.

  18. Standard Technical Specifications General Electric plants, BWR/4: Bases (Sections 2.0-3.3). Volume 2, Revision 1

    SciTech Connect

    1995-04-01

    This report documents the results of the combined effort of the NRC and the industry produce improved Standard Technical Specifications (STS), Revision 1 for General Electric BWR/4 Plants. The changes reflected in Revision 1 resulted from the experience gained from license amendment applications to convert to these improved ST or to adopt partial improvements to existing technical specifications. This NUREG is the result of extensive public technical meetings and discussions between the Nuclear Regulatory Commission (NRC) staff and various nuclear power plant licensees, Nuclear Steam Supply System (NSSS) Owners Groups, NSSS vendors, and the Nuclear Energy Institute (NEI). The improved STS were developed based on the criteria in the Final Commission Policy Statement on Technical Specifications Improvements for Nuclear Power Reactors, dated July 22, 1993. The improved STS will be used as the basis for individual nuclear power plant licensees to develop improved plant-specific technical specifications. This report contains three volumes. Volume I contains the Specifications for all chapters and sections of the improved STS. This document, Volume 2, contains the Bases for Chapters 2.0 and 3.0, and Sections 3.1-3.3 of the improved STS. Volume 3 contains the Bases for Sections 3.4-3.10 of the improved STS.

  19. Characterization of a New Organic-Cation Cyclotetraphosphate: (1,4-HOC 6H 4NH 3) 4P 4O 12· 6H 2O

    NASA Astrophysics Data System (ADS)

    Soumhi, E. H.; Saadoune, I.; Driss, A.; Jouini, T.

    1999-05-01

    The tetra(para-phenolammonium)cyclotetraphosphate hexahydrate, (1,4-HOC6H4NH3)4P4O12· 6H2O (M=864.51 g mol-1), is monoclinicP21/cwith the unit cell parametersa=9.836(2) Å,b=8.591(1) Å,c:22.769(5) Å,β=95.41(2)°. The structure of this compound can be described as a succession of inorganic and organic sheets parallel to the (001) plane. The existence of the OH and NH3groups in positionparato the organic cation leads to the cohesion of the inorganic sheets, forming a three-dimensional network.The IR spectrum of (1,4-HOC6H4NH3)4P4O12· 6H2O is reported and discussed according to the theoretical group analysis. The IR data confirm the atomic arrangement within the structure. The coupled TG-DTA thermal study shows the successive departure of four and two water molecules, confirming the hydrated character of this cyclophosphate.

  20. Palladium-catalyzed heteroannulation leading to heterocyclic structures with two heteroatoms: a highly regio- and stereoselective synthesis of (Z)-4-alkyl-2-alkyl(aryl)idene-3,4-dihydro-2H-1,4-benzoxazines and (Z)-3-alkyl(aryl)idene-4-tosyl-3,4-dihydro-2H-1,4-benzoxazines.

    PubMed

    Kundu, N G; Chaudhuri, G; Upadhyay, A

    2001-01-12

    A highly convenient method has been developed for the synthesis of (Z)-4-alkyl-2-alkyl(aryl)idene-3,4-dihydro-2H-1,4-benzoxazines 9 and (Z)-3-alkyl(aryl)idene-4-tosyl-3,4-dihydro-2H-1,4-benzoxazines 34-38 through palladium-copper-catalyzed reactions. Aryl halides 7 reacted with 2-[N-alkyl(benzyl)-N-prop-2'-ynyl]aminophenyl tosylate 6 in the presence of (PPh3)2PdCl2 (3 mol %), CuI(5 mol %) in triethylamine at room temperature to yield 2-[N-alkyl(benzyl)-N-(3-aryl-prop-2'-ynyl)]-aminophenyl tosylates 8 in extremely good yields (72-96%). The latter could then be cyclized with KOH in ethanol-water to Z-9 in a highly regio- and stereoselective manner. Similarly, palladium-copper-catalyzed reaction of 2-(prop-2'-ynyloxy)aniline (21) with aryl iodides 7 led to 22-26 which after tosylation and cyclization with cuprous iodide in CH3CN in the presence of K2CO3 and Bu4-NBr led to the (Z)-3-alkyl(aryl)idene-4-tosyl 3,4-dihydro-2H-1,4-benzoxazines 34-38 in good overall yields. The Z-stereochemistry of the products was established from 1H NMR spectra, 3JCH values (between vinylic proton and methylenic carbon of the heterocyclic ring), NOE experiments, and X-ray analysis. The method was also found to be suitable for the synthesis of bis(benzoxazinylated) derivatives 17, 39, and 2-alkyl-3,4-dihydro-2H-1,4-benzoxazines 18. Our method for the synthesis of 3,4-dihydro-2H-1,4-benzoxazines is highly efficacious, using easily available starting materials under very mild conditions. Also the synthesis of some novel 5-substituted uracil derivatives 40 and 41 containing the benzoxazinyl moiety and of potential biological interest is being reported.

  1. 40 CFR 721.5262 - 2,7-Naphthalenedisulfonic acid, 5-[[4-chloro-6-[substituted] amino]-1,3,5-triazin-2-yl]amino]-4...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...,7-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3- -, trisodium salt... identified generically as 2,7-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3... 40 Protection of Environment 30 2010-07-01 2010-07-01 false 2,7-Naphthalenedisulfonic acid,...

  2. 40 CFR 721.5262 - 2,7-Naphthalenedisulfonic acid, 5-[[4-chloro-6-[substituted] amino]-1,3,5-triazin-2-yl]amino]-4...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ...,7-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3- -, trisodium salt... identified generically as 2,7-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3... 40 Protection of Environment 32 2013-07-01 2013-07-01 false 2,7-Naphthalenedisulfonic acid,...

  3. 40 CFR 721.5262 - 2,7-Naphthalenedisulfonic acid, 5-[[4-chloro-6-[substituted] amino]-1,3,5-triazin-2-yl]amino]-4...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ...,7-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3- -, trisodium salt... identified generically as 2,7-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3... 40 Protection of Environment 32 2012-07-01 2012-07-01 false 2,7-Naphthalenedisulfonic acid,...

  4. 40 CFR 721.5262 - 2,7-Naphthalenedisulfonic acid, 5-[[4-chloro-6-[substituted] amino]-1,3,5-triazin-2-yl]amino]-4...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...,7-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3- -, trisodium salt... identified generically as 2,7-Naphthalenedisulfonic acid, 5- amino]-1,3,5-triazin-2-yl]amino]-4-hydroxy-3... 40 Protection of Environment 31 2011-07-01 2011-07-01 false 2,7-Naphthalenedisulfonic acid,...

  5. Comparison of thermal lensing effects between single-end and double-end diffusion-bonded Nd:YVO4 crystals for 4F 3/2-->4I 11/2 and 4F 3/2-->4I 13/2 transitions.

    PubMed

    Chang, Y T; Huang, Y P; Su, K W; Chen, Y F

    2008-12-08

    The effective focal lengths of thermal lens in diode-end-pumped continuous-wave Nd:YVO(4) lasers for the (4)F(3/2)-->(4)I(11/2) and (4)F(3/2)-->(4)I(13/2) transitions were determined. The experimental results revealed that the thermal lensing effect for the (4)F(3/2)-->(4)I(11/2) transition can be sufficiently improved by employing a single-end diffusion-bonded Nd:YVO(4) crystal replacing a conventional Nd:YVO(4) crystal. However, using a double-end diffusion-bonded Nd:YVO(4) crystal was a great improvement over a single-end diffusion-bonded Nd:YVO(4) crystal for the (4)F(3/2)-->(4)I(13/2) transition with stronger thermal lensing effect.

  6. Synthesis and Characterization of La 3NbSe 2O 4F 2

    NASA Astrophysics Data System (ADS)

    Brennan, Theodore D.; Mansuetto, Michael F.; Ibers, James A.

    1993-12-01

    Crystals of the unusual oxyfluoroselenide La 3NbSe 2O 4F 2 were obtained during the exploration of the quaternary La/Nb/Cu/Se system. Oxygen was extracted from the silica tube, while fluorine was present as a minor impurity in the La powder. The compound crystallizes in space group D 162 h- Pnma of the orthorhombic system with four formula units in a cell with dimensions: a = 11.290(4), b = 4.001(1), and c = 18.062(4) Å ( T = 113 K). The structure has been determined by single-crystal X-ray methods. The presence of F in the crystals was confirmed by windowless EDAX measurements. The two F sites were distinguished from the four O sites from a combination of the X-ray refinement and a bond-valence parameter calculation made with the program EUTAX. In the structure the Nb atom is octahedrally coordinated while each of the three independent La atoms is in a tricapped trigonal prism. The Nb atom is bound to one Se atom and five O atoms while the three La sites are coordinated by various combinations of Se, O, and F atoms. The NbO 5Se octahedra corner share and the LaSe xO yF z tricapped trigonal prisms face share in the b direction.

  7. Scale-4 Analysis of Pressurized Water Reactor Critical Configurations: Volume 2-Sequoyah Unit 2 Cycle 3

    SciTech Connect

    Bowman, S.M.

    1995-01-01

    The requirements of ANSI/ANS 8.1 specify that calculational methods for away-from-reactor criticality safety analyses be validated against experimental measurements. If credit for the negative reactivity of the depleted (or spent) fuel isotopics is desired, it is necessary to benchmark computational methods against spent fuel critical configurations. This report summarizes a portion of the ongoing effort to benchmark away-from-reactor criticality analysis methods using critical configurations from commercial pressurized-water reactors. The analysis methodology selected for all the calculations reported herein is based on the codes and data provided in the SCALE-4 code system. The isotopic densities for the spent fuel assemblies in the critical configurations were calculated using the SAS2H analytical sequence of the SCALE-4 system. The sources of data and the procedures for deriving SAS2H input parameters are described in detail. The SNIKR code module was used to extract the necessary isotopic densities from the SAS2H results and provide the data in the format required by the SCALE criticality analysis modules. The CSASN analytical sequence in SCALE-4 was used to perform resonance processing of the cross sections. The KENO V.a module of SCALE-4 was used to calculate the effective multiplication factor (k{sub eff}) of each case. The SCALE-4 27-group burnup library containing ENDF/B-IV (actinides) and ENDF/B-V (fission products) data was used for all the calculations. This volume of the report documents the SCALE system analysis of three reactor critical configurations for the Sequoyah Unit 2 Cycle 3. This unit and cycle were chosen because of the relevance in spent fuel benchmark applications: (1) the unit had a significantly long downtime of 2.7 years during the middle of cycle (MOC) 3, and (2) the core consisted entirely of burned fuel at the MOC restart. The first benchmark critical calculation was the MOC restart at hot, full-power (HFP) critical conditions. The

  8. Synthesis, characterization, and crystal structure of 2-amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[3,2- c]pyran-3-carbonitrile

    NASA Astrophysics Data System (ADS)

    Sharma, S.; Banerjee, B.; Brahmachari, G.; Kant, Rajni; Gupta, V. K.

    2015-12-01

    2-Amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[3,2- c]pyran-3-carbonitrile, C16H12N2O3 is synthesized via one-pot multi-component reaction at room temperature using commercially available urea as inexpensive and environmentally benign organo-catalyst. Its structure is determined by single-crystal X-ray diffraction technique The crystals are monoclinic, a = 10.7357(12), b = 8.7774(8), c = 15.0759(16) Å, β = 103.575(11)°, Z = 4, sp. gr. P21/ n, R = 0.0551 for 1696 observed reflections. The crystal structure is stabilized by N-H···N, C-H···O, and C-H···π interactions.

  9. BF3·Et2O Catalysed 4-Aryl-3-phenyl-benzopyrones, Pro-SERMs, and Their Characterization

    PubMed Central

    Srivastava, Ambika; Singh, Pooja; Kumar, Rajesh

    2015-01-01

    We have synthesized the novel 4-(4-hydroxy-benzyl)-3-phenyl-chromen-2-one which is a precursor of SERMs with a smaller number of steps and good yield. Two methodologies for the synthesis have been worked out. Anhydrous BF3·Et2O catalyzed reaction was found to be selective for product formation while anhydrous AlCl3, FeCl3, and SnCl4 catalyzed ones were nonselective. PMID:26421007

  10. Synthesis, antifungal activity and docking study of 2-amino-4H-benzochromene-3-carbonitrile derivatives

    NASA Astrophysics Data System (ADS)

    Mirjalili, BiBi Fatemeh; Zamani, Leila; Zomorodian, Kamiar; Khabnadideh, Soghra; Haghighijoo, Zahra; Malakotikhah, Zahra; Ayatollahi Mousavi, Seyyed Amin; Khojasteh, Shaghayegh

    2016-07-01

    Pathogenic fungi are associated with diseases ranging from simple dermatosis to life-threatening infections, particularly in immunocompromised patients. During the past two decades, resistance to established antifungal drugs has increased dramatically and has made it crucial to identify novel antimicrobial compounds. Here, we selected 12 new compounds of 2-amino-4H-benzochromene-3-carbonitrile drivetives (C1-C12) for synthesis by using nano-TiCl4.SiO2 as efficient and green catalyst, then nine of synthetic compounds were evaluated against different species of fungi, positive gram and negative gram of bacteria. Standard and clinical strains of antibiotics sensitive and resistant fungi and bacteria were cultured in appropriate media. Biological activity of the 2-amino-4H-benzochromene-3-carbonitrile derivatives against fungi and bacteries were estimated by the broth micro-dilution method as recommended by clinical and laboratory standard institute (CLSI). In addition minimal fangicidal and bactericial concenteration of the compounds were also determined. Considering our results showed that compound 2-amino-4-(4-methyl benzoate)-4H-benzo[f]chromen-3-carbonitrile (C9) had the most antifungal activity against Aspergillus clavatus, Candida glabarata, Candida dubliniensis, Candida albicans and Candida tropicalis at concentrations ranging from 8 to ≤128 μg/mL. Also compounds 2-amino-4-(3,4-dimethoxyphenyl)-4H-benzo[f]chromen-3-carbonitrile (C4) and 2-amino-4-(4-isopropylphenyl)-4H-benzo[f]chromen-3-carbonitrile (C3) had significant inhibitory activities against Epidermophyton floccosum following 2-amino-4-(4-methylbenzoate)-4H-benzo[f]chromen-3-carbonitrile (C9), respectively. Docking simulation was performed to insert compounds C3, C4 and C9 in to CYP51 active site to determine the probable binding model.

  11. 40 CFR 721.5281 - 2-Naphthalenesulfonic acid, 3-[[4-[(2,4-dimethyl-6-sulfophenyl)azo]-2-methoxy-5-methylphenyl]azo...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 32 2012-07-01 2012-07-01 false 2-Naphthalenesulfonic acid, 3- -2-methoxy-5-methylphenyl]azo]-4-hydroxy-7-(phenylamino)-, sodium salt, compd. With 2,2â²,2â³-nitrilotris (9CI). 721.5281 Section 721.5281 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT SIGNIFICANT...

  12. 40 CFR 721.5281 - 2-Naphthalenesulfonic acid, 3-[[4-[(2,4-dimethyl-6-sulfophenyl)azo]-2-methoxy-5-methylphenyl]azo...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 31 2011-07-01 2011-07-01 false 2-Naphthalenesulfonic acid, 3- -2-methoxy-5-methylphenyl]azo]-4-hydroxy-7-(phenylamino)-, sodium salt, compd. With 2,2â²,2â³-nitrilotris (9CI). 721.5281 Section 721.5281 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT SIGNIFICANT...

  13. 40 CFR 721.5281 - 2-Naphthalenesulfonic acid, 3-[[4-[(2,4-dimethyl-6-sulfophenyl)azo]-2-methoxy-5-methylphenyl]azo...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false 2-Naphthalenesulfonic acid, 3- -2-methoxy-5-methylphenyl]azo]-4-hydroxy-7-(phenylamino)-, sodium salt, compd. With 2,2â²,2â³-nitrilotris (9CI). 721.5281 Section 721.5281 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT SIGNIFICANT...

  14. 40 CFR 721.5281 - 2-Naphthalenesulfonic acid, 3-[[4-[(2,4-dimethyl-6-sulfophenyl)azo]-2-methoxy-5-methylphenyl]azo...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false 2-Naphthalenesulfonic acid, 3- -2-methoxy-5-methylphenyl]azo]-4-hydroxy-7-(phenylamino)-, sodium salt, compd. With 2,2â²,2â³-nitrilotris (9CI). 721.5281 Section 721.5281 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT SIGNIFICANT...

  15. 40 CFR 721.5281 - 2-Naphthalenesulfonic acid, 3-[[4-[(2,4-dimethyl-6-sulfophenyl)azo]-2-methoxy-5-methylphenyl]azo...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 32 2013-07-01 2013-07-01 false 2-Naphthalenesulfonic acid, 3- -2-methoxy-5-methylphenyl]azo]-4-hydroxy-7-(phenylamino)-, sodium salt, compd. With 2,2â²,2â³-nitrilotris (9CI). 721.5281 Section 721.5281 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT SIGNIFICANT...

  16. (2,2-Bipyridyl)bis(eta5-1,2,3,4,5-pentamethylcyclopentadienyl)Strontium(II)

    SciTech Connect

    Kazhdan, Daniel; Kazhdan, Daniel; Hu, Yung-Jin; Kokai, Akos; Levi, Zerubba; Rozenel, Sergio

    2008-07-03

    In the title compound, the Sr-N distances are 2.624 (3) and 2.676 (3) Angstroms. The Sr-centroid distances are 2.571 and 2.561 Angstroms. The N-C-C-N torsion angle in the bipyridine ligand is 2.2 (4){sup o}. Interestingly, the bipyridine ligand is tilted. The angle between the plane defined by Sr1, N1 and N2 and the plane defined by the 12 atoms of the bipyridine ligand is 10.7{sup o}.

  17. Synthesis in the Melt and Characterization of Condensed Binary Phosphates BaNH 4(PO 3) 3, BiNH 4P 4O 12, and Ti(NH 4) 2P 4O 13

    NASA Astrophysics Data System (ADS)

    Selevich, Anatoly F.; Levchik, Sergei V.; Lyakhov, Alexander S.; Levchik, Galina F.; Lesnikovich, Anatoly I.; Catala, Jean-Marie

    1996-08-01

    Barium-ammonium polyphosphate (BaNH4(PO3)3), bismuth-ammonium cyclotetraphosphate (BiNH4P4O12), and titanium-ammonium tetraphosphate (Ti(NH4)2P4O13) have been synthesized in the melt of ammonium polyphosphate (NH4PO3). The prepared phosphates were characterized by chemical analysis, thin layer chromatography, and X-ray diffraction of powders. BiNH4P4O12was found to crystallize in the cubic system, space groupI43dwith the unit-cell parametera= 15.105(2) Å. Thermal decomposition behavior of the phosphates was studied by thermogravimetry and crystalline products of degradation were identified.

  18. Comparison of the hydrogen-bond patterns in 2-amino-1,3,4-thiadiazolium hydrogen oxalate, 2-amino-1,3,4-thiadiazole-succinic acid (1/2), 2-amino-1,3,4-thiadiazole-glutaric acid (1/1) and 2-amino-1,3,4-thiadiazole-adipic acid (1/1).

    PubMed

    Matulková, Irena; Císařová, Ivana; Němec, Ivan; Fábry, Jan

    2014-10-01

    The X-ray single-crystal structure determinations of the chemically related compounds 2-amino-1,3,4-thiadiazolium hydrogen oxalate, C2H4N3S(+)·C2HO4(-), (I), 2-amino-1,3,4-thiadiazole-succinic acid (1/2), C2H3N32C4H6O4, (II), 2-amino-1,3,4-thiadiazole-glutaric acid (1/1), C2H3N3S·C5H8O4, (III), and 2-amino-1,3,4-thiadiazole-adipic acid (1/1), C2H3N3S·C6H10O4, (IV), are reported and their hydrogen-bonding patterns are compared. The hydrogen bonds are of the types N-H···O or O-H···N and are of moderate strength. In some cases, weak C-H···O interactions are also present. Compound (II) differs from the others not only in the molar ratio of base and acid (1:2), but also in its hydrogen-bonding pattern, which is based on chain motifs. In (I), (III) and (IV), the most prominent feature is the presence of an R2(2)(8) graph-set motif formed by N-H···O and O-H···N hydrogen bonds, which are present in all structures except for (I), where only a pair of N-H···O hydrogen bonds is present, in agreement with the greater acidity of oxalic acid. There are nonbonding S···O interactions present in all four structures. The difference electron-density maps show a lack of electron density about the S atom along the S···O vector. In all four structures, the carboxylic acid H atoms are present in a rare configuration with a C-C-O-H torsion angle of ∼0°. In the structures of (II)-(IV), the C-C-O-H torsion angle of the second carboxylic acid group has the more common value of ∼|180|°. The dicarboxylic acid molecules are situated on crystallographic inversion centres in (II). The Raman and IR spectra of the title compounds are presented and analysed.

  19. Nature of phase transitions in ammonium oxofluorovanadates, a vibrational spectroscopy study of (NH4)3VO2F4 and (NH4)3VOF5

    NASA Astrophysics Data System (ADS)

    Gerasimova, Yu. V.; Oreshonkov, A. S.; Laptash, N. M.; Vtyurin, A. N.; Krylov, A. S.; Shestakov, N. P.; Ershov, A. A.; Kocharova, A. G.

    2017-04-01

    Two ammonium oxofluorovanadates, (NH4)3VO2F4 and (NH4)3VOF5, have been investigated by temperature-dependent infrared and Raman spectroscopy methods to determine the nature of phase transitions (PT) in these compounds. Dynamics of quasioctahedral groups was simulated within the framework of semi-empirical approach, which justified the cis-conformation of VO2F43 - (C2v) and the C4v geometry of VOF53 -. The observed infrared and Raman spectra of both compounds at room temperature (RT) revealed the presence at least of two crystallographically independent octahedral groups. The first order PT at elevated temperatures is connected with a complete dynamic disordering of these groups with only single octahedral state. At lower temperatures, the octahedra are ordered and several octahedral states appear. This PT is the most pronounced in the case of (NH4)3VOF5, when at least seven independent VOF53 - octahedra are present in the structure below 50 K, in accordance with the Raman spectra. Ammonium groups do not take part in PTs at higher and room temperatures but their reorientational motion freezes at lower temperatures.

  20. Practical and Efficient Synthesis of α-Aminophosphonic Acids Containing 1,2,3,4-Tetrahydroquinoline or 1,2,3,4-Tetrahydroisoquinoline Heterocycles.

    PubMed

    Ordóñez, Mario; Arizpe, Alicia; Sayago, Fracisco J; Jiménez, Ana I; Cativiela, Carlos

    2016-08-31

    We report here a practical and efficient synthesis of α-aminophosphonic acid incorporated into 1,2,3,4-tetrahydroquinoline and 1,2,3,4-tetrahydroisoquinoline heterocycles, which could be considered to be conformationally constrained analogues of pipecolic acid. The principal contribution of this synthesis is the introduction of the phosphonate group in the N-acyliminium ion intermediates, obtained from activation of the quinoline and isoquinoline heterocycles or from the appropriate δ-lactam with benzyl chloroformate. Finally, the hydrolysis of phosphonate moiety with simultaneous cleavage of the carbamate afforded the target compounds.

  1. T(T,2n)4He and 3He(3He,2p)4He: The Reaction Mechanism from Solar Energies to 10 MeV

    NASA Astrophysics Data System (ADS)

    Bacher, A. D.; Brune, C. R.; Sayre, D. B.; Hale, G. M.; Frenje, J. A.; Gatu Johnson, M.

    2016-03-01

    We have studied the energy dependence of the reaction mechanism of the T(t,2n)4He reaction at stellar energies and of its charge symmetric analog reaction 3He(3He,2p)4He at energies up 10 MeV. We find that the reaction mechanism changes dramatically over this energy range in part due to the interference of the two identical fermions in the three-body final state. This contribution is dedicated to the memory of Tom Tombrello, my Ph.D. advisor at Cal Tech, who died in 2014.

  2. Hydrothermal synthesis of In2S3/g-C3N4 heterojunctions with enhanced photocatalytic activity.

    PubMed

    Xing, Chaosheng; Wu, Zhudong; Jiang, Deli; Chen, Min

    2014-11-01

    Graphitic carbon nitride (g-C3N4) was hybridized by In2S3 to form a novel In2S3/g-C3N4 heterojunction photocatalyst via a hydrothermal method. TEM and HRTEM results reveal that In2S3 nanoparticles and g-C3N4 closely contact with each other to form an intimate interface. The as-obtained In2S3/g-C3N4 heterojunctions exhibit higher photocatalytic activity than those of pure g-C3N4 and In2S3 for the photodegradation of rhodamine B (RhB) under visible light irradiation. The enhanced photocatalytic performance of In2S3/g-C3N4 heterojunctions could be attributed to its wide absorption in the visible region and efficient electron-hole separation. On the basis of radical scavenger experiments, superoxide radicals and holes are suggested to play a critical role in RhB degradation over In2S3/g-C3N4 heterojunctions.

  3. Synthesis and Electrochemical Performance of the Na3V2(PO4)3 Cathode for Sodium-Ion Batteries

    NASA Astrophysics Data System (ADS)

    Van Nghia, Nguyen; Jafian, Samuel; Hung, I.-Ming

    2016-05-01

    Rhombohedral Na3V2(PO4)3 with a Na+ superionic conductor structure was synthesized using a solid-state reaction method. Citric acid was used as a carbon resource for carbon-thermal reduction reaction to reduce the oxidation state of vanadium. The shape of Na3V2(PO4)3 particles is irregular and its average diameter is in the range 30-50 nm. The Na3V2(PO4)3 exhibits a superior cycling ability and rate capability. The discharge capacity retains 74.3% of the discharge capacity of its first cycle with coulombic efficiency of 99.3% after 100 cycles. The discharge capacity of Na3V2(PO4)3 at 10 C is 48.87 mAh g-1, which is 58.4% of the cell cycled at 0.1 C. Furthermore, the structure of Na3V2(PO4)3 is stable for a considerable amount of Na+ ions (2 mol of Na+ ions) insertion and extraction with only 0.42% difference of unit-cell volume between fully charged and discharged states. Na3V2(PO4)3 is a potential cathode material for sodium-ion battery applications.

  4. RELAP5-3D Developmental Assessment: Comparison of Versions 4.3.4i and 4.2.1i

    SciTech Connect

    Bayless, Paul David

    2015-10-01

    Figures have been generated comparing the parameters used in the developmental assessment of the RELAP5-3D code using versions 4.3.4i and 4.2.1i. The figures, which are the same as those used in Volume III of the RELAP5-3D code manual, compare calculations using the semi-implicit solution scheme with available experiment data. These figures provide a quick, visual indication of how the code predictions changed between these two code versions and can be used to identify cases in which the assessment judgment may need to be changed in Volume III of the code manual. Changes to the assessment judgments made after reviewing all of the assessment cases are also provided.

  5. 2-[4-Acetyl-5-(biphenyl-4-yl)-4,5-dihydro-1,3,4-oxadiazol-2-yl]phenyl acetate

    PubMed Central

    Yehye, Wagee A.; Ariffin, Azhar; Rahman, Noorsaadah Abdul; Ng, Seik Weng

    2010-01-01

    In the title mol­ecule, C24H20N2O4, the five-membered oxadiazole ring is nearly planar (r.m.s. deviation = 0.053 Å) and the phenyl ring of the biphenyl unit attached to it forms a dihedral angle of 73.2 (1)°; the other phenyl ring is close to coplanar with the oxadiazole ring [dihedral angle = 6.2 (2)°]. PMID:21580697

  6. Luminescence Spectra of ZnAl 2 O 4 {:}Cr 3+ Spinel Nanopowders

    NASA Astrophysics Data System (ADS)

    Luc, H. H.; Nguyen, T. K.; Nguyen, V. M.; Suchocki, A.; Kamiñska, A.; Le, V. K.; Nguyen, V. H.; Luong, T. T.

    2002-12-01

    The synthetic ZnAl 2 O 4 spinels doped with Cr 3+ ions are prepared from ZnSO,dwi{4}>, Al 2 (SO 4 ) 3 , and Cr 2 (SO 4 ) 3 . The spinel single phase is detected from X-ray diffraction. Luminescence properties of Cr 3+ in ZnAl 2 O 4 were studied by low temperature luminescence and decay measurements. Four luminescence lines at 14570, 14520, 14460, and 14330 cm -1 were found to originate from structure distortion and the line at 14175 cm -1 - from chromium pairs. The broad emission band at about 13540 cm -1 is considered to arise from a new Cr 3+ center in ZnCr 2 O 4 .

  7. 5-(Adamantan-1-yl)-3-[(4-benzyl­piperazin-1-yl)meth­yl]-1,3,4-oxadiazole-2(3H)-thione

    PubMed Central

    El-Emam, Ali A.; El-Brollosy, Nasser R.; Attia, Mohamed I.; Said-Abdelbaky, Mohammed; García-Granda, Santiago

    2012-01-01

    The mol­ecule of the title compound, C24H32N4OS, is a functionalized 1,3,4-oxadiazole-2-thione with substituted piperazine and adamantanyl substituents attached at the 3- and 5-positions, respectively, of the oxadiazole spacer with an approximately C-shaped conformation. In the crystal, mol­ecules form dimers via C—H⋯S inter­action. The piperazine ring has a chair conformation; the substituents S, methyl­ene C and adamantane C of the essentially planar oxadiazole ring are approximately in the same plane, with distances of −0.046 (2), −0.085 (5) and 0.003 (4) Å, respectively. The dihedral angle between the planes of the phenyl and oxadiazole rings is 31.3 (3)°. PMID:22798843

  8. Be3(AsO4)2 2H2O, a New Berylloarsenate Phase Containing Bridged Tetrahedral 3-Rings

    DTIC Science & Technology

    1994-04-15

    CsH(ZnPO 4 )2 and NaH(ZnPO 4 )2 contain "bridged" 3-rings as part of anionic layers sandwiching cesium and sodium cations (9). Finally, the novel...0 have been found in the layered, anionic zincophosphate phases CsH(ZnPO 4 )2 and NaH(ZnP0 4 )2 (9). However, the precise nature of the tetrahedral

  9. Dichloridobis[3-(4-meth­oxy­phen­yl)-2-methyl-5-(piperidin-1-yl)-2,3-di­hydro-1,2,4-oxa­diazole-κN 4]platinum(II)

    PubMed Central

    Kritchenkov, Andreii S.; Lavnevich, Leonid V.; Starova, Galina L.; Bokach, Nadezhda A.; Kalibabchuk, Valentina A.

    2013-01-01

    In title compound, [PtCl2(C15H21N3O2)2], the PtII cation, located on an inversion center, is coordinated by two Cl− anions and two 3-(4-meth­oxy­phen­yl)-2-methyl-5-(piperidin-1-yl)-2,3-di­hydro-1,2,4-oxa­diazole ligands in a distorted Cl2N2 square-planar geometry. The di­hydro­oxa­diazole and piperidine rings display envelope (with the non-coordinating N atom as the flap atom) and chair conformations, respectively. In the crystal, weak C—H⋯Cl hydrogen bonds link the mol­ecules into supra­molecular chains running along the b axis. The piperidine ring is disordered over two positions with the occupancy ratio of 0.528 (4):0.472 (4). PMID:24109266

  10. Vicarious nucleophilic substitution using 4-amino-1,2,4-triazole, hydroxylamine or O-alkylhydroxylamine to prepare 1,3-diamino-2,4,6-trinitrobenzene or 1,3,5-triamino-2,4,6-trinitrobenzene

    DOEpatents

    Mitchell, A.R.; Pagoria, P.F.; Schmidt, R.D.

    1997-05-27

    The present invention relates to a process to produce 1,3-diamino-2,4,6-trinitrobenzene (DATB) or 1,3,5-triamino-2,4,6,trinitrobenzene (TATB) by: (a) reacting at ambient pressure and a temperature of between about 0 and 50 C for between about 0.1 and 24 hr, a trinitroaromatic compound of the structure shown where X, Y, and Z are each independently selected from the group consisting of -H and -NH{sub 2}, with the proviso that at least 1 or 2 of X, Y, and Z are hydrogen; with an effective amount of 1-amino-1,2,4-triazole, hydroxylamine or O-alkylhydroxamine to produce DATB or TATB; in the presence of a strong base selected from sodium butoxide, potassium butoxide, potassium propoxide, sodium propoxide, sodium ethoxide, potassium ethoxide, sodium methoxide, potassium methoxide, and combinations thereof; in a solvent selected from the group consisting of methanol, ethanol, propanol, butanol, dimethylsulphoxide, N-methylpyrrolidone, hexamethylphosphoramide, dimethylformide, dimethylacetamide and mixtures thereof, provided that when alcohols are present or when hydroxylamine or its O-alkyl derivatives replace ATA primarily DATB is formed; and (b) isolating the DATB or TATB produced. DATB and TATB are important and useful specialty explosives and intermediates for other materials.

  11. Vicarious nucleophilic substitution using 4-amino-1,2,4-triazole, hydroxylamine or O-alkylhydroxylamine to prepare 1,3-diamino-2,4,6-trinitrobenzene or 1,3,5-triamino-2,4,6-trinitrobenzene

    DOEpatents

    Mitchell, Alexander R.; Pagoria, Philip F.; Schmidt, Robert D.

    1997-01-01

    The present invention relates to a process to produce 1,3-diamino-2,4,6-trinitrobenzene (DATB) or 1,3,5-triamino-2,4,6,-trinitrobenzene (TATB) by: (a) reacting at ambient pressure and a temperature of between about 0.degree. and 50.degree. C. for between about 0.1 and 24 hr, a trinitroaromatic compound of structure V: ##STR1## wherein X, Y, and Z are each independently selected from the group consisting of --H and --NH.sub.2, with the proviso that at least 1 or 2 of X, Y, and Z are hydrogen; with an effective amount of 1-amino-1,2,4-triazole, hydroxylamine or O-alkylhydroxamine to produce DATB or TATB; in the presence of a strong base selected from sodium butoxide, potassium butoxide, potassium propoxide, sodium propoxide, sodium ethoxide, potassium ethoxide, sodium methoxide, potassium methoxide, and combinations thereof; in a solvent selected from the group consisting of methanol, ethanol, propanol, butanol, dimethylsulphoxide, N-methylpyrrolidone, hexamethylphosphoramide, dimethylformide, dimethylacetamide and mixtures thereof, provided that when alcohols are present or when hydroxylamine or its O-alkyl derivatives replace ATA primarily DATB is formed; and (b) isolating the DATB or TATB produced. DATB and TATB are important and useful specialty explosives and intermediates for other materials.

  12. Measurement of OH, H2SO4, MSA, and HNO3 Aboard the P-3B Aircraft

    NASA Technical Reports Server (NTRS)

    Eisele, F. L.

    2003-01-01

    This paper addresses the measurement of OH, H2SO4, MSA, and HNO3 aboard the P-3B aircraft under the following headings: 1) Performance Report; 2) Highlights of OH, H2SO4, and MSA Measurements Made Aboard the NASA P-3B During TRACE-P; 3) Development and characteristics of an airborne-based instrument used to measure nitric acid during the NASA TRACE-P field experiment.

  13. THE STRUCTURE, MAGNETISM AND CONDUCTIVITY OF Li3V2(PO4)3: A THEORETICAL AND EXPERIMENTAL STUDY

    NASA Astrophysics Data System (ADS)

    Lin, Zhi-Ping; Zhao, Yu-Jun; Zhao, Yan-Ming

    2013-10-01

    In this paper, we present a combination of first-principles and experimental investigations on the structural, magnetic and electronic properties of monoclinic Li3V2(PO4)3. The change of dielectric constant indicates that the structural phase transition appear around the temperature 120°C. The first-principles calculation and magnetic measurement display that Li3V2(PO4)3 is a compound with weak ferromagnetism, with Curie constant of C = 0.004 and Curie temperature of 140 K. The experimental and theoretical results demonstrated that the Li3V2(PO4)3 is a typical semiconductor.

  14. Thermal quenching of luminescence of LiSr4 (BO3)3:Eu2+ orange-emitting phosphor.

    PubMed

    Zhang, Xinguo; Zhou, Liya; Gong, Menglian

    2014-03-01

    An orange-emitting phosphor, Eu(2+)-activated LiSr4(BO3)3, was synthesized using the conventional solid-state reaction. The photoluminescence excitation and emission spectra, and temperature dependence of the luminescence intensity of the phosphor were investigated. The results showed that LiSr4(BO3)3:Eu(2+) could be efficiently excited by incident light of 250-450 nm, and emits a strong orange light. With increasing temperature, the emission bands of LiSr4(BO3)3:Eu(2+) show an abnormal blue-shift with broadening bandwidth and decreasing emission intensity.

  15. Antimicrobial activity of quinoxaline 1,4-dioxide with 2- and 3-substituted derivatives.

    PubMed

    Vieira, Mónica; Pinheiro, Cátia; Fernandes, Rúben; Noronha, João Paulo; Prudêncio, Cristina

    2014-04-01

    Quinoxaline is a chemical compound that presents a structure that is similar to quinolone antibiotics. The present work reports the study of the antimicrobial activity of quinoxaline N,N-dioxide and some derivatives against bacterial and yeast strains. The compounds studied were quinoxaline-1,4-dioxide (QNX), 2-methylquinoxaline-1,4-dioxide (2MQNX), 2-methyl-3-benzoylquinoxaline-1,4-dioxide (2M3BenzoylQNX), 2-methyl-3-benzylquinoxaline-1,4-dioxide (2M3BQNX), 2-amino-3-cyanoquinoxaline-1,4-dioxide (2A3CQNX), 3-methyl-2-quinoxalinecarboxamide-1,4-dioxide (3M2QNXC), 2-hydroxyphenazine-N,N-dioxide (2HF) and 3-methyl-N-(2-methylphenyl)quinoxalinecarboxamide-1,4-dioxide (3MN(2MF)QNXC). The prokaryotic strains used were Staphylococcus aureus ATCC 6538, S. aureus ATCC 6538P, S. aureus ATCC 29213, Escherichia coli ATCC 25922, E. coli S3R9, E. coli S3R22, E. coli TEM-1 CTX-M9, E. coli TEM-1, E. coli AmpC Mox-2, E. coli CTX-M2 e E. coli CTX-M9. The Candida albicans ATCC 10231 and Saccharomyces cerevisiae PYCC 4072 were used as eukaryotic strains. For the compounds that presented activity using the disk diffusion method, the minimum inhibitory concentration (MIC) was determined. The alterations of cellular viability were evaluated in a time-course assay. Death curves for bacteria and growth curves for S. cerevisiae PYCC 4072 were also accessed. The results obtained suggest potential new drugs for antimicrobial activity chemotherapy since the MIC's determined present low values and cellular viability tests show the complete elimination of the bacterial strain. Also, the cellular viability tests for the eukaryotic model, S. cerevisiae, indicate low toxicity for the compounds tested.

  16. Microwave sol-gel synthesis and upconversion photoluminescence properties of CaGd2(WO4)4:Er3+/Yb3+ phosphors with incommensurately modulated structure

    NASA Astrophysics Data System (ADS)

    Lim, Chang Sung; Aleksandrovsky, Aleksandr; Molokeev, Maxim; Oreshonkov, Aleksandr; Atuchin, Victor

    2015-08-01

    CaGd2-x(WO4)4:Er3+/Yb3+ phosphors with the doping concentrations of Er3+ and Yb3+ (x=Er3++Yb3+, Er3+=0.05, 0.1, 0.2 and Yb3+=0.2, 0.45) have been successfully synthesized by the microwave sol-gel method. The crystal structure of CaGd2-x(WO4)4:Er3+/Yb3+ tungstates have been refined, and upconversion photoluminescence properties have been investigated. The synthesized particles, being formed after the heat-treatment at 900 °C for 16 h, showed a well crystallized morphology. Under the excitation at 980 nm, CaGd2(WO4)4:Er3+/Yb3+ particles exhibited a strong 525-nm and a weak 550-nm emission bands in the green region and a very weak 655-nm emission band in the red region. The Raman spectrum of undoped CaGd2(WO4)4 revealed about 12 narrow lines. The strongest band observed at 903 cm-1 was assigned to the ν1 symmetric stretching vibration of WO4 tetrahedrons. The spectra of the samples doped with Er and Yb obtained under the 514.5 nm excitation were dominated by Er3+ luminescence preventing the recording of these samples Raman spectra. Concentration quenching of the erbium luminescence at 2H11/24I15/2 transition is weak in the range of erbium doping level xEr=0.05-0.2, while, for transition 4S3/24I15/2, the signs of concentration quenching become pronounced at xEr=0.2.

  17. Synthesis and evaluation of 8-amino-[1,2,4]triazolo[4,3-a]pyridin-3(2H)-one derivatives as glycogen synthase kinase-3 (GSK-3) inhibitors.

    PubMed

    Chun, Kwangwoo; Park, Ji-Seon; Lee, Han-Chang; Kim, Young-Ha; Ye, In-Hea; Kim, Kang-Jeon; Ku, Il-Whea; Noh, Min-Young; Cho, Goang-Won; Kim, Heejaung; Kim, Seung Hyun; Kim, Jeongmin

    2013-07-01

    New potent glycogen synthase kinase-3 (GSK-3) inhibitors, 8-amino-[1,2,4]triazolo[4,3-a]pyridin-3(2H)-one derivatives, were designed by modeling, synthesized and evaluated in vitro. Compound 17c showed good potency in enzyme and cell-based assays (IC50=111 nM, EC50=1.78 μM). Moreover, it has demonstrated desirable water solubility, PK profile, and moderate brain penetration.

  18. (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol inhibits growth of colon tumors in mice.

    PubMed

    Zheng, Jie; Park, Mi Hee; Son, Dong Ju; Choi, Min Gi; Choi, Jeong Soon; Nam, Kyung Tak; Kim, Hae Deun; Rodriguez, Kevin; Gann, Benjamin; Ham, Young Wan; Han, Sang Bae; Hong, Jin Tae

    2015-12-08

    In our previous study, we found that (E)-2,4-bis(p-hydroxyphenyl)-2-butenal showed anti-cancer effect, but it showed lack of stability and drug likeness. We have prepared several (E)-2,4-bis(p-hydroxyphenyl)-2-butenal analogues by Heck reaction. We selected two compounds which showed significant inhibitory effect of colon cancer cell growth. Thus, we evaluated the anti-cancer effects and possible mechanisms of one compound (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol in vitro and in vivo. In this study, we found that (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol induced apoptotic cell death in a dose dependent manner (0-15 μg/ml) through activation of Fas and death receptor (DR) 3 in HCT116 and SW480 colon cancer cell lines. Moreover, the combination treatment with (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol and nuclear factor κB (NF-κB) inhibitor, phenylarsine oxide (0.1 μM) or signal transducer and activator of transcription 3 (STAT3) inhibitor, Stattic (50 μM) increased the expression of Fas and DR3 more significantly. In addition, (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol suppressed the DNA binding activity of both STAT3 and NF-κB. Knock down of STAT3 or NF-κB p50 subunit by STAT3 small interfering RNA (siRNA) or p50 siRNA magnified (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol-induced inhibitory effect on colon cancer cell growth. Besides, the expression of Fas and DR3 was increased in STAT3 siRNA or p50 siRNA transfected cells. Moreover, docking model and pull-down assay showed that (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol directly bound to STAT3 and NF-κB p50 subunit. Furthermore, (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol inhibited colon tumor growth in a dose dependent manner (2.5 mg/kg-5 mg/kg) in mice. Therefore, these findings indicated that (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol may be a promising anti-cancer agent for colon cancer with more advanced research.

  19. (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol inhibits growth of colon tumors in mice

    PubMed Central

    Son, Dong Ju; Choi, Min Gi; Choi, Jeong Soon; Nam, Kyung Tak; Kim, Hae Deun; Rodriguez, Kevin; Gann, Benjamin; Ham, Young Wan; Han, Sang Bae; Hong, Jin Tae

    2015-01-01

    In our previous study, we found that (E)-2,4-bis(p-hydroxyphenyl)-2-butenal showed anti-cancer effect, but it showed lack of stability and drug likeness. We have prepared several (E)-2,4-bis(p-hydroxyphenyl)-2-butenal analogues by Heck reaction. We selected two compounds which showed significant inhibitory effect of colon cancer cell growth. Thus, we evaluated the anti-cancer effects and possible mechanisms of one compound (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol in vitro and in vivo. In this study, we found that (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol induced apoptotic cell death in a dose dependent manner (0-15 μg/ml) through activation of Fas and death receptor (DR) 3 in HCT116 and SW480 colon cancer cell lines. Moreover, the combination treatment with (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol and nuclear factor κB (NF-κB) inhibitor, phenylarsine oxide (0.1 μM) or signal transducer and activator of transcription 3 (STAT3) inhibitor, Stattic (50 μM) increased the expression of Fas and DR3 more significantly. In addition, (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol suppressed the DNA binding activity of both STAT3 and NF-κB. Knock down of STAT3 or NF-κB p50 subunit by STAT3 small interfering RNA (siRNA) or p50 siRNA magnified (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol-induced inhibitory effect on colon cancer cell growth. Besides, the expression of Fas and DR3 was increased in STAT3 siRNA or p50 siRNA transfected cells. Moreover, docking model and pull-down assay showed that (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol directly bound to STAT3 and NF-κB p50 subunit. Furthermore, (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol inhibited colon tumor growth in a dose dependent manner (2.5 mg/kg-5 mg/kg) in mice. Therefore, these findings indicated that (E)-4-(3-(3,5-dimethoxyphenyl)allyl)-2-methoxyphenol may be a promising anti-cancer agent for colon cancer with more advanced research. PMID

  20. Heterogeneous reactions of NO2 with CaCO3-(NH4)2SO4 mixtures at different relative humidities

    NASA Astrophysics Data System (ADS)

    Tan, Fang; Tong, Shengrui; Jing, Bo; Hou, Siqi; Liu, Qifan; Li, Kun; Zhang, Ying; Ge, Maofa

    2016-07-01

    In this work, the heterogeneous reactions of NO2 with CaCO3-(NH4)2SO4 mixtures with a series of weight percentage (wt %) of (NH4)2SO4 were investigated using diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) at different relative humidity (RH) values. For comparison, the heterogeneous reactions of NO2 with pure CaCO3 particles and pure (NH4)2SO4 particles, as well as the reaction of CaCO3 with (NH4)2SO4 particles, were also studied. The results indicated that NO2 did not show any significant uptake on (NH4)2SO4 particles, and it reacted with CaCO3 particles to form calcium nitrate under both dry and wet conditions. The heterogeneous reactions of NO2 with CaCO3-(NH4)2SO4 mixtures were markedly dependent on RH. Calcium nitrate was formed from the heterogeneous reactions at all the RHs investigated, whereas CaSO4 ṡ 0.5H2O (bassanite), CaSO42H2O (gypsum), and (NH4)2Ca(SO4)2 ṡ H2O (koktaite) were produced depending on RH. Under the dry condition, the heterogeneous uptake of NO2 on the mixtures was similar to that on CaCO3 particles with neglectable effects from (NH4)2SO4; the duration of initial stages and the NO3- mass concentrations had a negative linear relation with the mass fraction of (NH4)2SO4 in the mixtures. Under wet conditions, the chemical interaction of (NH4)2SO4 with Ca(NO3)2 enhances the nitrate formation, especially at medium RHs, while the coagulation of (NH4)2SO4 with CaCO3 exhibits an increasing inhibiting effects with increasing RH at the same time. In addition, the heterogeneous uptake of NO2 on the mixtures of CaCO3 and (NH4)2SO4 was found to favor the formation of bassanite and gypsum due to the decomposition of CaCO3 and the coagulation of Ca2+ and SO42-. A possible reaction mechanism was proposed and the atmospheric implications were discussed.

  1. Etude des transitions de phases de NH 3(CH 2) 2NH 3(H 2PO 4) 2 par mesures optique, dielectrique et de thermocourant

    NASA Astrophysics Data System (ADS)

    Kamoun, S.; Daoud, A.; Von Der Muhll, R.; Ravez, J.

    1993-02-01

    Dielectric, birefringence and thermocurrent measurements have been carried out on NH 3(CH 2) 2NH 3(H 2PO 4) 2 single crystal. Three transitions have been detected at about T 1 = (264 + 4), T 2 = (241 + 5) and T 3 = (141 + 5) K. In the low temperature phases a polarization current of about 10 -8 - 10 -9 A is obtained and can be reversed when the sign of the polarization field is changed, a property which could correspond to a ferroelectric behaviour. However, no pyroelectric current is detected when the temperature decreases from T t. Another hypothesis, based on a field - induced polarization, has been considered : the depolarization current could be due to charge displacements from potential minima favored by rising temperature. In any way, the low - temperature phases are characterized by a remanent polarization.

  2. New 1-(3-nitrophenyl)-5,6-dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepines: synthesis and computational study.

    PubMed

    Kosychova, Lidija; Karalius, Antanas; Staniulytė, Zita; Sirutkaitis, Romualdas Aleksas; Palaima, Algirdas; Laurynėnas, Audrius; Anusevičius, Žilvinas

    2015-03-26

    Triazole derivatives constitute an important group of heterocyclic compounds have have been the subject of extensive study in the recent past. These compounds have shown a wide range of biological and pharmacological activities. In this work, new fused tricyclic 1-(3-nitrophenyl)-5,6-dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]-benzodiazepines have been synthesized by the thermal cyclization of N'-(2,3-dihydro-1H-1,5-benzodiazepin-4-yl)-3-nitrobenzohydrazides. After screening ethanol, toluene and 1-butanol as solvents, butanol-1 was found to be the best choice for the cyclization reaction in order to obtain the highest yields of tricyclic derivatives. The chemical structures of the synthesized compounds were elucidated by the analysis of their IR, 1H- and 13C-NMR spectral data. For tentative rationalization of the reaction processes, the global and local reactivity indices of certain compounds, taking part in the reaction pathway, were assessed by means of quantum mechanical calculations using the conceptual density functional theory (DFT) approach. This work could be useful for the synthesis of new heterocyclic compounds bearing a fused triazole ring.

  3. Synthesis and structure of spiro[2-(2-methylphenyl)-4H-1,3-benzoxazine-4,2′-adamantane

    SciTech Connect

    Osyanin, V. A. Ivleva, E. A.; Rybakov, V. B.; Klimochkin, Yu. N.

    2015-01-15

    Synthesis and an X-ray diffraction study of spiro[2-(2-methylphenyl)-4H-1,3-benzoxazine-4,2′-adamantane] C{sub 24}H{sub 25}NO are performed: monoclinic crystal system, space group P2{sub 1}/c, a = 13.9424(3) Å, b = 7.56554(17) Å, c = 17.0155(3) Å, β = 99.6457(18)°, Z = 4, V = 1769.45(6) Å{sup 3}. ρ{sub calcd} = 1.244 g/cm{sup 3}, R = 0.0339 [T = 100(2) K]. The oxazine ring of the molecule adopts the boat conformation. The bond lengths and angles are standard for this class of compounds.

  4. [Theoretical and experimental vibrational spectroscopy study of K3Ln(PO4)2 phosphates].

    PubMed

    Benarafa, L; Rghioui, L; Nejjar, R; Saidi Idrissi, M; Knidiri, M; Lorriaux, A; Wallart, F

    2005-01-14

    The monoclinic phosphates with K3Ln(PO4)2 (Ln=rare earth) formula were synthesized. Their infrared and Raman spectra have been reported and analysed. The results of a force field calculation for K3Nd(PO4)2 are presented.

  5. The Big E (Energy). 4-H Leader's Guide for Units 2 & 3.

    ERIC Educational Resources Information Center

    Caldwell, William; And Others

    This leader's guide is designed for units 2 and 3 of the Nebraska 4-H Energy Project. The goals of the project are to: (1) help young people understand energy problems related to life styles; (2) use energy resources carefully; (3) guide members in choosing their own energy alternatives; and (4) to enjoy together the challenges and creativity of…

  6. The PtdIns(3,4)P(2) phosphatase INPP4A is a suppressor of excitotoxic neuronal death.

    PubMed

    Sasaki, Junko; Kofuji, Satoshi; Itoh, Reietsu; Momiyama, Toshihiko; Takayama, Kiyohiko; Murakami, Haruka; Chida, Shinsuke; Tsuya, Yuko; Takasuga, Shunsuke; Eguchi, Satoshi; Asanuma, Ken; Horie, Yasuo; Miura, Kouichi; Davies, Elizabeth Michele; Mitchell, Christina; Yamazaki, Masakazu; Hirai, Hirokazu; Takenawa, Tadaomi; Suzuki, Akira; Sasaki, Takehiko

    2010-05-27

    Phosphorylated derivatives of phosphatidylinositol, collectively referred to as phosphoinositides, occur in the cytoplasmic leaflet of cellular membranes and regulate activities such as vesicle transport, cytoskeletal reorganization and signal transduction. Recent studies have indicated an important role for phosphoinositide metabolism in the aetiology of diseases such as cancer, diabetes, myopathy and inflammation. Although the biological functions of the phosphatases that regulate phosphatidylinositol-3,4,5-trisphosphate (PtdIns(3,4,5)P(3)) have been well characterized, little is known about the functions of the phosphatases regulating the closely related molecule phosphatidylinositol-3,4-bisphosphate (PtdIns(3,4)P(2)). Here we show that inositol polyphosphate phosphatase 4A (INPP4A), a PtdIns(3,4)P(2) phosphatase, is a suppressor of glutamate excitotoxicity in the central nervous system. Targeted disruption of the Inpp4a gene in mice leads to neurodegeneration in the striatum, the input nucleus of the basal ganglia that has a central role in motor and cognitive behaviours. Notably, Inpp4a(-/-) mice show severe involuntary movement disorders. In vitro, Inpp4a gene silencing via short hairpin RNA renders cultured primary striatal neurons vulnerable to cell death mediated by N-methyl-d-aspartate-type glutamate receptors (NMDARs). Mechanistically, INPP4A is found at the postsynaptic density and regulates synaptic NMDAR localization and NMDAR-mediated excitatory postsynaptic current. Thus, INPP4A protects neurons from excitotoxic cell death and thereby maintains the functional integrity of the brain. Our study demonstrates that PtdIns(3,4)P(2), PtdIns(3,4,5)P(3) and the phosphatases acting on them can have distinct regulatory roles, and provides insight into the unique aspects and physiological significance of PtdIns(3,4)P(2) metabolism. INPP4A represents, to our knowledge, the first signalling protein with a function in neurons to suppress excitotoxic cell death

  7. Infrared spectroscopic method for analysis of Mg 2Ca(SO 4) 3 in mixtures with MgSO 4 and/or CaSO 4

    NASA Astrophysics Data System (ADS)

    Smith, Duane H.; Seshadri, Kal S.

    1999-04-01

    Mg 2Ca(SO 4) 3 is prepared from, and may be found in, mixtures with MgSO 4 and CaSO 4. Such mixtures frequently occur in the ash produced by various types of coal combustion, especially in filter cakes from pressurized fluidized bed combustion with dolomite as a SO x sorbent. Previously, qualitative analyses could be performed for Mg 2Ca(SO 4) 3 in these mixtures, but no quantitative analytical method was available. An infrared spectroscopic method has been developed that provides reasonably quantitative results for Mg 2Ca(SO 4) 3, MgSO 4,and CaSO 4 in their mixtures.

  8. Redetermination of kovdorskite, Mg2PO4(OH)·3H2O

    PubMed Central

    Morrison, Shaunna M.; Downs, Robert T.; Yang, Hexiong

    2012-01-01

    The crystal structure of kovdorskite, ideally Mg2PO4(OH)·3H2O (dimagnesium phosphate hydroxide trihydrate), was reported previously with isotropic displacement paramaters only and without H-atom positions [Ovchinnikov et al. (1980 ▶). Dokl. Akad. Nauk SSSR. 255, 351–354]. In this study, the kovdorskite structure is redetermined based on single-crystal X-ray diffraction data from a sample from the type locality, the Kovdor massif, Kola Peninsula, Russia, with anisotropic displacement parameters for all non-H atoms, with all H-atom located and with higher precision. Moreover, inconsistencies of the previously published structural data with respect to reported and calculated X-ray powder patterns are also discussed. The structure of kovdorskite contains a set of four edge-sharing MgO6 octa­hedra inter­connected by PO4 tetra­hedra and O—H⋯O hydrogen bonds, forming columns and channels parallel to [001]. The hydrogen-bonding system in kovdorskite is formed through the water mol­ecules, with the OH− ions contributing little, if any, to the system, as indicated by the long H⋯A distances (>2.50 Å) to the nearest O atoms. The hydrogen-bond lengths determined from the structure refinement agree well with Raman spectroscopic data. PMID:22346789

  9. Redetermination of kovdorskite, Mg(2)PO(4)(OH)·3H(2)O.

    PubMed

    Morrison, Shaunna M; Downs, Robert T; Yang, Hexiong

    2012-02-01

    The crystal structure of kovdorskite, ideally Mg(2)PO(4)(OH)·3H(2)O (dimagnesium phosphate hydroxide trihydrate), was reported previously with isotropic displacement paramaters only and without H-atom positions [Ovchinnikov et al. (1980 ▶). Dokl. Akad. Nauk SSSR.255, 351-354]. In this study, the kovdorskite structure is redetermined based on single-crystal X-ray diffraction data from a sample from the type locality, the Kovdor massif, Kola Peninsula, Russia, with anisotropic displacement parameters for all non-H atoms, with all H-atom located and with higher precision. Moreover, inconsistencies of the previously published structural data with respect to reported and calculated X-ray powder patterns are also discussed. The structure of kovdorskite contains a set of four edge-sharing MgO(6) octa-hedra inter-connected by PO(4) tetra-hedra and O-H⋯O hydrogen bonds, forming columns and channels parallel to [001]. The hydrogen-bonding system in kovdorskite is formed through the water mol-ecules, with the OH(-) ions contributing little, if any, to the system, as indicated by the long H⋯A distances (>2.50 Å) to the nearest O atoms. The hydrogen-bond lengths determined from the structure refinement agree well with Raman spectroscopic data.

  10. Up-conversion emission in KGd(WO 4 ) 2 single crystals triply-doped with Er 3+ /Yb 3+ /Tm 3+ , Tb 3+ /Yb 3+ /Tm 3+ and Pr 3+ /Yb 3+ /Tm 3+ ions

    NASA Astrophysics Data System (ADS)

    Kasprowicz, D.; Brik, M. G.; Majchrowski, A.; Michalski, E.; Głuchowski, P.

    2011-09-01

    Triply-doped single crystals KGd(WO 4) 2:Er 3+/Yb 3+/Tm 3+, KGd(WO 4) 2:Tb 3+/Yb 3+/Tm 3+ and KGd(WO 4) 2:Pr 3+/Yb 3+/Tm 3+ were grown by the Top Seeded Solution Growth (TSSG) method, with an aim of getting efficient up-converted multicolored luminescence, which subsequently can be used for generation of white light. Such an aim determined the choice of the triply doped compounds: excitation of the Yb 3+ ions in the infrared spectral region is followed by red, green and blue emission from other dopants. It was shown that all these systems exhibit multicolor up-conversion fluorescence under 980 nm laser irradiation. Detailed spectroscopic studies of their absorption and luminescence spectra were performed. From the analysis of the dependence of the intensity of fluorescence on the excitation power the conclusion was made about significant role played by the host's conduction band and other possible defects of the KGd(WO 4) 2 crystal lattice in the up-conversion processes.

  11. Synthesis and anti-inflammatory activity evaluation of some novel 6-alkoxy(phenoxy)-[1,2,4]triazolo[3,4-a]phthalazine-3-amine derivatives.

    PubMed

    Sun, Xian-Yu; Hu, Chuan; Deng, Xian-Qing; Wei, Cheng-Xi; Sun, Zhi-Gang; Quan, Zhe-Shan

    2010-11-01

    Starting from phthalic anhydride, several new 6-alkoxy(phenoxy)-[1,2,4]triazolo[3,4-a]phthalazine-3-amine derivatives were synthesized as potent anti-inflammatory agent. The study showed that the compounds 6h (6-(2-chlorophenoxy)-[1,2,4]triazolo[3,4-a]phthalazine-3-amine) and 6s (6-(4-aminophenoxy)-[1,2,4] triazolo[3,4-a]phthalazine-3-amine) exhibited the highest anti-inflammatory activity (81% and 83% inhibition, respectively, at 0.5 h after i.p. administration) which were slightly more potent than the reference drug Ibuprofen (61%). Furthermore, the peak activity of 6h and 6s was observed at the 3 h after p.o. administration, and they exhibited stronger anti-inflammatory activity than Ibuprofen at the dose of 50 mg/kg at the peak time.

  12. Vibrational Spectra of 3-(Adamantan-1-YL)-4-(2-Propen-1-YL)-1 H-1,2,4-Triazole-5(4 H)-Thione

    NASA Astrophysics Data System (ADS)

    Gladkov, L. L.; Matsukovich, A. S.; Pavich, T. A.; Gaponenko, S. V.; El-Emam, A. A.

    2017-01-01

    Vibrational spectra of 3-(adamantan-1-yl)-4-(2-propen-1-yl)-1H-1,2,4-triazole-5(4H)-thione (C15H21N3S), which was promising for drug development, were studied experimentally and theoretically. The geometric structure and normal modes of the molecule and its dimer were calculated using quantum-mechanical density functional theory. It was shown that the experimentally obtained vibrational spectra were due to dimeric C15H21N3S structures. This conclusion was confirmed by spectra of the isotopically substituted compound with a deuterated imine. Bands at 1496 and 1549 cm-1 were identified as markers of dimer formation. Bands at 936 and 1244 cm-1 were found to be markers of intermolecular interactions of adamantane fragments.

  13. Tris(2-ethylamino)amine ( tren) as template for the elaboration of fluorides: synthesis and crystal structures of [(C 2H 4NH 3) 3NH]·[Zr 3F 16(H 2O)], [(C 2H 4NH 3) 3N] 2·[ZrF 6]·[Zr 2F 12] and [(C 2H 4NH 3) 3N]·[TaF 7]·F

    NASA Astrophysics Data System (ADS)

    Goreshnik, E.; Leblanc, M.; Maisonneuve, V.

    2004-11-01

    Using tris(2-ethylamino)amine ( tren) as a template, three new fluorides are obtained by solvothermal synthesis: [(C 2H 4NH 3) 3NH]·[Zr 3F 16(H 2O)] ( I), [(C 2H 4NH 3) 3N] 2·[ZrF 6]·[Zr 2F 12] ( II) and [(C 2H 4NH 3) 3N]·[TaF 7]·F ( III). The structure determinations are performed by single crystal technique. The structure of I consists of infinite spiral-like [Zr 3F 16(H 2O)] 4- chains connected by tetraprotonated [ trenH 4] 4+ cations which possess a plane configuration. In II, isolated [ZrF 6] octahedra or [Zr 2F 12] dimers are linked to organic cations by a tridimensional hydrogen bond network. In III, [TaF 7] 2- monocapped trigonal prisms and "isolated" fluoride ions are connected by hydrogen bonds to template moieties. In II and III, every organic moiety is triprotonated [ trenH 3] 3+ with a "spider" configuration. In the tantalum phase, the hydrogen bond network leads to the formation of a layered structure.

  14. Fused polycyclic compounds via cycloaddition of 4-(1'-cyclohexenyl)-5-iodo-1,2,3-triazoles with 4-phenyl-1,2,4-triazoline-3,5-dione: the importance of a sacrificial iodide leaving group.

    PubMed

    Michaels, Heather A; Simmons, J Tyler; Clark, Ronald J; Zhu, Lei

    2013-05-17

    4-(1'-Cyclohexenyl)-5-iodo-1,2,3-triazole and 4-phenyl-1,2,4-triazoline-3,5-dione undergo a formal Diels-Alder reaction, which following an S(N)2' solvolysis process to displace the iodo group affords a fused polycyclic compound.

  15. Solid state synthesis and tunable luminescence of Li2SrSiO4:Eu2+/Ce3+ phosphors

    NASA Astrophysics Data System (ADS)

    Wei, Zhen; Wang, Yongli; Zhu, Xiaobo; Guan, Jinyu; Mao, Weixi; Song, Juanjuan

    2016-03-01

    Li2SrSiO4:Eu2+/Ce3+ phosphors have been synthesized by solid state reaction. Eu2+ and/or Ce3+ doped Li2SrSiO4 have the hexagonal crystal structure, indicating the doped Eu2+ and/or Ce3+ ions have no influence on the crystal structure of Li2SrSiO4. Under the excitation at 365 nm, Eu2+ or Ce3+ doped Li2SrSiO4 phosphors give characteristic emission bands of Eu2+ or Ce3+, respectively. For Li2SrSiO4:Eu2+/Ce3+ phosphors with the fixed Ce3+ concentration, two emission bands originating from Eu2+ and Ce3+ can be observed. On the basis of luminescent properties of Li2SrSiO4:Eu2+/Ce3+ phosphors, we can conclude that energy transfer from Ce3+ to Eu2+ occurs in Li2SrSiO4.

  16. Synthesis of 2',4-dihydroxy-3-methoxychalcone and 2',4',4-trihydroxy-3-methoxychalcone as a candidate anticancer against cervical (WiDr), colon (HeLa), and breast (T47d) cancer cell lines in vitro

    NASA Astrophysics Data System (ADS)

    Matsjeh, Sabirin; Swasono, Respati Tri; Anwar, Chairil; Solikhah, Eti Nurwening; Lestari, Endang

    2017-03-01

    The compound 2',4-dihydroxy-3-methoxychalcone and 2',4',4-trihydroxy-3-methoxychalcone have been synthesized through Claisen-Schmidt reaction from 2-hydroxyacetophenone and 2,4-dihydroxyacetophenone with 4-hydroxy-3-methoxy benzaldehida (vanillin) in aqueous KOH 40% and KSF montmorillonite as catalyst in methanol. All these products were characterized by FT-IR, TLC Scanner, GC-MS, MS-Direct, and 1H-NMR and 13C-NMR spectrometer. Both of these compounds were tested citotoxycity activity as an anticancer against cervical, colon, and breast cancer cells (Hela, WiDr, and T47D cell lines) using MTT assay in vitro. Dose series given test solution concentration on Hela, WiDr, and T47D cells started from 6,25; 25; 50 and 100 µg/mL with incubation treatment for 24 hours. The result of study showed that the 2',4-dihydroxy-3-methoxychalcone as bright yellow crystal with the melting point of 114-115 °C and the yield of 13.77% and the 2',4',4-trihydroxy-3-methoxychalcone as bright yellow crystals with the melting point of 195-197 °C and the yield of 6%. Other 2',4-dihydroxy-3-methoxychalcone and 2',4',4-trihydroxy-3-methoxychalcone also exhibited cytotoxic activity against the cancer cell lines, with the 2',4',4-trihydroxy-3-methoxychalcone showed greater activities than the 2',4-dihydroxy-3-methoxychalcone in WiDr cell lines. The 2',4-dihydroxy-3-methoxychalcone and 2',4',4-trihydroxy-3-methoxychalcone exhibited strong anticancer activities with IC50 value below 20 µg/mL. The activity of 2',4',4-trihydroxy-3-methoxychalcone showed the most active against Hela and WiDr cell lines with IC50 value 8.53 and 2.66 µg/mL respectively, than T47D cell lines with IC50 value 24.61 µg/mL. The test results cytotoxic of 2',4-dihydroxy-3-methoxychalcone showed the most active against Hela and WiDr cell lines with IC50 value 12.80, 19.57 µg/mL than T47D cell lines with IC50 value of 20.73 µg/mL. IC50 value indicated that 2',4-dihydroxy-3-methoxychalcone and 2',4',4-trihydroxy-3

  17. Structural and computational characterization of 4‧,4‧,6‧,6‧-tetrachloro-3-(2-methoxyethyl)-3H,4H-spiro-1,3,2-benzoxaza phosphinine-2,2‧- [1,3,5,2,4,6] triazatriphosphinine

    NASA Astrophysics Data System (ADS)

    Işıklan, Muhammet; Yıldırım, Erdem Kamil; Atiş, Murat; Sonkaya, Ömer; Çoşut, Bünyemin

    2016-08-01

    In this study a new monospirocyclic phosphazene derivative, 4‧,4‧,6‧,6‧-tetrachloro-3-(2-methoxyethyl)-3H,4H-spiro [1,3,2-benzoxazaphosphinine-2,2‧- [1,3,5,2,4,6] triazatriphosphinine] (SP1) was synthesized from the reaction of hexachlorocyclotriphosphazene (N3P3Cl6) with N/O donor-type, 2-{[(2-Metoxyethyl) amino]methyl}phenol. The structural investigations of the compound were verified by elemental analyses, MS, FTIR, 1H, 13C, 31P NMR spectroscopy and the single crystal X-ray diffraction analysis. The structural and spectroscopic data of the molecule in the ground state were calculated by using density functional method (DFT) using 6-311++G (d, p) basis set. The complete assignments of all vibrational modes were performed on the basis of the total energy distributions (TED). Isotropic chemical shifts (31P, 1H and 13C NMR) were calculated using the gauge-invariant atomic orbital (GIAO) method. Theoretical calculations of bond parameters, harmonic vibration frequencies and nuclear magnetic resonance are in good agreement with experimental results. The electrophilic and nucleophilic attack centers in SP1 were predicted with the local softness values (sk+, and sk-) of individual atoms and it is confirmed that P atoms of the PCl2 groups are nucleophilic attack centers.

  18. 9-Furfuryl-idene-2,3-dimethyl-6,7,8,9-tetrahydro-4H--thieno[2',3':4,5]pyrimidino[1,2-a]pyridin-4-one.

    PubMed

    Bozorov, Khurshed A; Elmuradov, Burkhon Zh; Okmanov, Rasul Ya; Tashkhodjaev, Bakhodir; Shakhidoyatov, Khusnutdin M

    2010-02-06

    The title compound, C(17)H(16)N(2)O(2)S, was obtained by condensation of 2,3-dimethyl-thieno[2',3':4,5]pyrimidino[1,2-a]pyridin-4-one with furfural in the presence of sodium hydroxide. One of the methyl-ene groups of the tetra-hydro-pyrido ring is disordered over two positions in a 0.87 (1):0.13 (1) ratio. The thieno[2,3-d]pyrimidin-4-one unit and the furan ring are both planar (r.m.s. deviation = 0.535 Å), and coplanar with each other, forming a dihedral angle of 5.4 (1)°. Four weak inter-molecular hydrogen bonds (C-H⋯O and C-H⋯N) are observed in the structure, which join mol-ecules into a network parallel to (101).

  19. Discovery of novel 1,2,3,4-tetrahydrobenzo[4, 5]thieno[2, 3-c]pyridine derivatives as potent and selective CYP17 inhibitors.

    PubMed

    Wang, Mingliang; Fang, Yanjia; Gu, Shoulai; Chen, Fangfang; Zhu, Zhengjiang; Sun, Xun; Zhu, Jidong

    2017-03-21

    The inhibition of CYP17 to block androgen biosynthesis is a well validated strategy for the treatment of prostate cancer. Herein we reported the design, synthesis and structure-activity relationship (SAR) study for a series of novel 1,2,3,4- tetrahydrobenzo[4,5]thieno[2,3-c]pyridine derivatives. Some analogs demonstrated a potent inhibition to both rat and human CYP17 protein and reduced testosterone production in human H295R cell line. Some analogs also showed high selectivity against other CYP enzymes such as 3A4, 1A2, 2C9, 2C19 and 2D6, which may limit side effects due to drug-drug interactions. Among these analogs, the most potent compound 9c showed 1.5 fold more potent against rat and human CYP17 protein than that of abiraterone (IC50 = 16 nM and 20 nM vs. 25 nM and 36 nM respectively). In NCI-H295R cells, the inhibitory effect of compound 9c on testosterone production (52± 2%) was also more potent than that of abiraterone (74± 15%) at the concentration of 1 μM. Further, it was shown that 9c reduced plasma testosterone level in a dose-dependent manner in Sprague-Dawley rats. Thus, analog 9c maybe a potential agent used for the treatment of prostate cancer.

  20. POLY-1,2,4-TRIAZOLES AND POLY-1,3,4-OXADIAZOLES FROM PRECURSOR POLY-N-ACYLHYDRAZIDINES,

    DTIC Science & Technology

    oxadiazole . Whereas, conversion of the precursor poly-N-acylhydrazidine predominantly to poly-1,2,4-triazole was affected by refluxing in solvents such... oxadiazole depending upon the heating rate. Poly-N-acylhydrazidine was of sufficient molecular weight to cast a clear yellow film which exhibited good...flexibility. The film, upon thermal treatment to temperatures as high as 300C, became brittle. The poly-1,3,4- oxadiazole and poly-1,2,4-triazole

  1. Structural definition of the active site and catalytic mechanism of 3,4-dihydroxy-2-butanone-4-phosphate synthase.

    PubMed

    Liao, Der-Ing; Zheng, Ya-Jun; Viitanen, Paul V; Jordan, Douglas B

    2002-02-12

    X-ray crystal structures of L-3,4-dihydroxy-2-butanone-4-phosphate synthase from Magnaporthe grisea are reported for the E-SO(4)(2-), E-SO(4)(2-)-Mg(2+), E-SO(4)(2)(-)-Mn(2+), E-SO(4)(2)(-)-Mn(2+)-glycerol, and E-SO(4)(2)(-)-Zn(2+) complexes with resolutions that extend to 1.55, 0.98, 1.60, 1.16, and 1.00 A, respectively. Active-site residues of the homodimer are fully defined. The structures were used to model the substrate ribulose 5-phosphate in the active site with the phosphate group anchored at the sulfate site and the placement of the ribulose group guided by the glycerol site. The model includes two Mg(2+) cations that bind to the oxygen substituents of the C2, C3, C4, and phosphate groups of the substrate, the side chains of Glu37 and His153, and water molecules. The position of the metal cofactors and the substrate's phosphate group are further stabilized by an extensive hydrogen-bond and salt-bridge network. On the basis of their proximity to the substrate's reaction participants, the imidazole of an Asp99-His136 dyad from one subunit, the side chains of the Asp41, Cys66, and Glu174 residues from the other subunit, and Mg(2+)-activated water molecules are proposed to serve specific roles in the catalytic cycle as general acid-base functionalities. The model suggests that during the 1,2-shift step of the reaction, the substrate's C3 and C4 hydroxyl groups are cis to each other. A cis transition state is calculated to have an activation barrier that is 2 kcal/mol greater than that of the trans transition state in the absence of the enzyme.

  2. Structural definition of the active site and catalytic mechanism of 3,4-dihydroxy-2-butanone 4-phosphate synthase

    SciTech Connect

    Liao, D.-I.; Zheng, Y.-J.; Viitanen, P.V.; Jordan, D.B.

    2010-03-08

    X-ray crystal structures of L-3,4-dihydroxy-2-butanone-4-phosphate synthase from Magnaporthe grisea are reported for the E-SO{sub 4}{sup 2-}, E-{sub 4}{sup 2-}-Mg{sup 2+}, E-SO{sub 4}{sup 2-}-Mn{sup 2+}, E-SO{sub 4}{sup 2-}-Mn{sup 2+}-glycerol, and E-SO{sub 4}{sup 2-}-Zn{sup 2+} complexes with resolutions that extend to 1.55, 0.98, 1.60, 1.16, and 1.00 {angstrom}, respectively. Active-site residues of the homodimer are fully defined. The structures were used to model the substrate ribulose 5-phosphate in the active site with the phosphate group anchored at the sulfate site and the placement of the ribulose group guided by the glycerol site. The model includes two Mg{sup 2+} cations that bind to the oxygen substituents of the C2, C3, C4, and phosphate groups of the substrate, the side chains of Glu37 and His153, and water molecules. The position of the metal cofactors and the substrate's phosphate group are further stabilized by an extensive hydrogen-bond and salt-bridge network. On the basis of their proximity to the substrate's reaction participants, the imidazole of an Asp99-His136 dyad from one subunit, the side chains of the Asp41, Cys66, and Glu174 residues from the other subunit, and Mg{sup 2+}-activated water molecules are proposed to serve specific roles in the catalytic cycle as general acid-base functionalities. The model suggests that during the 1,2-shift step of the reaction, the substrate's C3 and C4 hydroxyl groups are cis to each other. A cis transition state is calculated to have an activation barrier that is 2 kcal/mol greater than that of the trans transition state in the absence of the enzyme.

  3. Regioselective synthesis of 2-amino-substituted 1,3,4-oxadiazole and 1,3,4-thiadiazole derivatives via reagent-based cyclization of thiosemicarbazide intermediate.

    PubMed

    Yang, Seung-Ju; Lee, Seok-Hyeong; Kwak, Hyun-Jung; Gong, Young-Dae

    2013-01-18

    A regioselective, reagent-based method for the cyclization reaction of 2-amino-1,3,4-oxadiazole and 2-amino-1,3,4-thiadiazole core skeletons is described. The thiosemicarbazide intermediate 3 was reacted with EDC·HCl in DMSO or p-TsCl, triethylamine in N-methyl-2-pyrrolidone to give the corresponding 2-amino-1,3,4-oxadiazoles 4 and 2-amino-1,3,4-thiadiazoles 5 through regioselcective cyclization processes. The regioselectivity was affected by both R(1) and R(2) in p-TsCl mediated cyclization. It is shown in select sets of thiosemicarbazide 3 with R(1)(benzyl) and R(2)(phenyl). 2-Amino-1,3,4-oxadiazole 4 was also shown in the reaction of p-TsCl mediated cyclization. The resulting 2-amino-1,3,4-oxadiazole and 2-amino-1,3,4-thiadiazole core skeleton are functionalized with various electrophiles such as alkyl halide, acid halides, and sulfornyl chloride in high yields.

  4. Effect of tyrphostin AG879 on Kv4.2 and Kv4.3 potassium channels

    PubMed Central

    Yu, Haibo; Zou, Beiyan; Wang, Xiaoliang; Li, Min

    2015-01-01

    Background and Purpose A-type potassium channels (IA) are important proteins for modulating neuronal membrane excitability. The expression and activity of Kv4.2 channels are critical for neurological functions and pharmacological inhibitors of Kv4.2 channels may have therapeutic potential for Fragile X syndrome. While screening various compounds, we identified tyrphostin AG879, a tyrosine kinase inhibitor, as a Kv4.2 inhibitor from. In the present study we characterized the effect of AG879 on cloned Kv4.2/Kv channel-interacting protein 2 (KChIP2) channels. Experimental Approach To screen the library of pharmacologically active compounds, the thallium flux assay was performed on HEK-293 cells transiently-transfected with Kv4.2 cDNA using the Maxcyte transfection system. The effects of AG879 were further examined on CHO-K1 cells expressing Kv4.2/KChIP2 channels using a whole-cell patch-clamp technique. Key Results Tyrphostin AG879 selectively and dose-dependently inhibited Kv4.2 and Kv4.3 channels. In Kv4.2/KChIP2 channels, AG879 induced prominent acceleration of the inactivation rate, use-dependent block and slowed the recovery from inactivation. AG879 induced a hyperpolarizing shift in the voltage-dependence of the steady-state inactivation of Kv4.2 channels without apparent effect on the V1/2 of the voltage-dependent activation. The blocking effect of AG879 was enhanced as channel inactivation increased. Furthermore, AG879 significantly inhibited the A-type potassium currents in the cultured hippocampus neurons. Conclusion and Implications AG879 was identified as a selective and potent inhibitor the Kv4.2 channel. AG879 inhibited Kv4.2 channels by preferentially interacting with the open state and further accelerating their inactivation. PMID:25752739

  5. Structures of two precursors to organic charge-transfer salts: 1,3-dithiolo[4,5-b][1,4]dithlin-2-thione and 1,3-dithiolo[4.5-b] [1,4]dithilin-2-one

    SciTech Connect

    Beno, M.A.; Kini, A.M.; Williams, J.M.

    1990-09-01

    C{sub 5}H{sub 4}S{sub 4}O (1), M{sub r} = 208.343, monoclinic, P2{sub 1}/n, a = 6.664 (2), b = 16.535 (6), c = 7.281 (2) {angstrom}, {beta} = 97.84 (3), V = 794.8 (5) {angstrom}{sup 3}, Z = 4, D{sub x} = 1.741 Mg m{sup {minus}3}, {lambda} (MoK{alpha}) = 0.71073 {angstrom}, {mu} = 1.07 mm{sup {minus}1}, F(000) = 424, T = 298 K, R(F) = 0.048 for 2338 reflections. C{sub 5}H{sub 4}S{sub 5} (2), M{sub r} = 224.39, monoclinic, P2{sub 1}/n, a = 10.765 (2), b = 5.879 (2), c = 13.479 (2) {angstrom}, {beta} = 92.66 (2), V = 852.2 (4) {angstrom}{sup 3}, Z = 4, D{sub x} = 1.749 Mg m{sup {minus}3}, {lambda} (MoK{alpha}) = 0. 71073 {angstrom}, {mu} = 1.23 mm{sup {minus}1}, F(000) = 456, T = 298 K, R(F) = 0.059 for 2491 reflections. Structure determinations for intermediates 1 and 2 were undertaken as part of a qualitative theoretical study of the changes in the geometries of organic donor molecules which occur with charge transfer. Although the geometries of 1 and 2 are nearly identical, the packing of these molecules in the unit cells is quite different. The molecular packing patterns are undoubtedly related to differences in the C-H{hor_ellipsis}chalcogen interactions for the thio and keto substituents.

  6. Synthesis and biological activity of cocaine analogues. 2. 6H-[2]Benzopyrano[4,3-c]pyridin-6-ones.

    PubMed

    Lazer, E S; Hite, G J; Nieforth, K A; Stratford, E S

    1979-07-01

    1,2,3,4-Tetrahydro-2-methyl-6H-[2]benzopyrano[4,3-c]pyridin-6-one (20) and cis- and trans-1,2,3,4,4a,10b-hexahydro-2-methyl-6H-[2]benzopyrano[4,3-c]pyridin-6-one (3a and 3b) were synthesized. The design of 3b was based on the proposal that the active conformation of cocaine is one in which the phenyl and amino groups are arranged in a manner that will superimpose upon a beta-phenethylamine in a trans-staggered conformation. The compounds were compared with cocaine and tropacocaine for their ability to inhibit uptake of [3H]norepinephrine by rat brain synaptosomal preparations. The test compounds (IC50 = 3.2 X 10(-4) M, 20; 6.5 X 10(-4) M, 3a; and 3.2 X 10(-4) M, 3b; respectively) were considerably weaker than cocaine (IC50 = 5.8 X 10(-7) M) and tropacocaine (IC50 = 5.6 X 10(-6) M). Compound 3b showed selectivity at 1 X 10(-5) M for inhibiting the uptake of norepinephrine (36%). It inhibited dopamine (3%) and serotonin (0%) uptake to a much lesser extent, if at all, at this concentration.

  7. Analogues of the muscarinic agent 2'-methylspiro[1-azabicyclo[2.2.2]octane-3,4'-[1,3]dioxolane]: synthesis and pharmacology.

    PubMed

    Nordvall, G; Sundquist, S; Glas, G; Gogoll, A; Nilvebrant, L; Hacksell, U

    1992-05-01

    A number of tetrahydrofuran analogues of 2'-methylspiro[1-azabicyclo[2.2.2]octane-3,4'-[1,3]dioxolane] (1) have been prepared with the aim to obtain information about the relative importance of each of the oxygens in 1 for efficacy and for selectivity. In addition, the dimethyl and desmethyl analogues of 1 were prepared. The new compounds were compared to cis- and trans-1 with regard to their ability to displace (-)-[3H]-3-quinuclidinyl benzilate ((-)-[3H]QNB) from muscarinic receptors in cerebral cortex, heart, parotid gland, and urinary bladder from guinea pigs. Functional studies were made on isolated guinea pig bladder and ileum. The new compounds exhibited both lower affinity and efficacy than cis-1. A conformational study was performed, and the effects of steric and electronic factors on the biological activity of the compounds are discussed.

  8. (3R,4S)-3-[4-(4-fluorophenyl)-4-hydroxypiperidin-1-yl]chroman-4,7-diol: a conformationally restricted analogue of the NR2B subtype-selective NMDA antagonist (1S,2S)-1-(4-hydroxyphenyl)-2-(4-hydroxy-4-phenylpiperidino)- 1-propanol.

    PubMed

    Butler, T W; Blake, J F; Bordner, J; Butler, P; Chenard, B L; Collins, M A; DeCosta, D; Ducat, M J; Eisenhard, M E; Menniti, F S; Pagnozzi, M J; Sands, S B; Segelstein, B E; Volberg, W; White, W F; Zhao, D

    1998-03-26

    (1S,2S)-1-(4-Hydroxyphenyl)-2-(4-hydroxy-4-phenylpiperidino)-1-propanol (CP-101,606, 1) is a recently described antagonist of N-methyl-D-aspartate (NMDA) receptors containing the NR2B subunit. In the present study, the optimal orientation of compounds of this structural type for their receptor was explored. Tethering of the pendent methyl group of 1 to the phenolic aromatic ring via an oxygen atom prevents rotation about the central portion of the molecule. Several of the new chromanol compounds have high affinity for the racemic [3H]CP-101,606 binding site on the NMDA receptor and protect against glutamate toxicity in cultured hippocampal neurons. The new ring caused a change in the stereochemical preference of the receptor-cis (erythro) compounds had better affinity for the receptor than the trans isomers. Computational studies suggest that steric interactions between the pendent methyl group and the phenol ring in the acyclic series determine which structures can best fit the receptor. The chromanol analogue, (3R,4S)-3-[4-(4-fluorophenyl)-4-hydroxypiperidin-1- yl]chroman-4,7-diol (12a, CP-283,097), was found to possess potency and selectivity comparable to CP-101,606. Thus 12a is a new tool to explore the function of the NR2B-containing NMDA receptors.

  9. Near-ultraviolet absorption spectra and crystal-field analysis of Gd3+ in Na3[Gd(C4H4O5)3].2NaClO4.6H2O

    NASA Astrophysics Data System (ADS)

    Stephens, Eileen M.; Metcalf, David H.; Berry, Mary T.; Richardson, F. S.

    1991-11-01

    Optical absorption spectra between 32 000 and 41 000 cm-1 are reported for Gd3+ in trigonal Na3[Gd(oxydiacetate)3].2NaClO4.6H2O at temperatures between 10 and 298 K. Fifty-eight of the 63 crystal-field levels split out of the 6PJ(J=7/2, 5/2, and 3/2), 6IJ(J=7/2, 9/2, 17/2, 11/2, 15/2, and 13/2), and 6DJ(J=9/2, 1/2, 7/2, 3/2, and 5/2) multiplets of the Gd3+ 4f7 electronic configuration are located and assigned from the low-temperature spectra, and these energy levels are analyzed in terms of a parametrized Hamiltonian that reflects D3 site symmetry at the Gd3+ ions. Parametric fits of calculated to empirical-energy-level data yield a rms deviation of 6.3 cm-1 (between calculated and observed energies). Eigenvectors of the parametrized Hamiltonian are used in calculations of oscillator strengths for all transitions that originate from the 8S7/2 (ground) multiplet and terminate on crystal-field levels of the 6PJ, 6IJ, and 6DJ multiplet manifolds. Spectra simulations based on these calculated oscillator strengths are presented, and comparisons between the simulated spectra and experimentally observed spectra show excellent agreement with respect to intensity distributions both within and between the various multiplet-to-multiplet transition manifolds. Variable-temperature absorption measurements carried out between 10 and 298 K showed only very small changes in J-multiplet baricenter energies, crystal-field-splitting energies (within J-multiplet manifolds), and transition intensity distributions. Disparities between the energy-level structure deduced in the present study and that proposed in another recently published study of Na3[Gd(oxydiacetate)3].2NaClO4.6H2O [Phys. Rev. B 41, 10 911 (1990)] are discussed. This previous study of Kundu, Banerjee, and Chowdhury was based on two-photon luminescence excitation measurements that have special significance for elucidating two-photon-absorption intensity mechanisms of 4f-4f transitions in noncentrosymmetric lanthanide

  10. 2-Sulfanylidene-1,3-dithiolo[4,5-b]naphtho­[2,3-e][1,4]dithiine-5,10-dione

    PubMed Central

    Méndez-Rojas, Miguel Angel; Bernès, Sylvain; Pérez-Benítez, Aarón; Romero Zarazúa, María Fernanda; Castellanos-Uribe, Adrián

    2011-01-01

    The title mol­ecule, C13H4O2S5, is folded by 47.83 (6)° along the S⋯S vector of the [1,4]dithiine six-membered ring, with the naphtho­quinone and [1,3]dithiole-2-thione moieties being nearly planar [largest deviations from least-squares planes = 0.028 (2) and 0.016 (1) Å, respectively]. This boat conformation is close to that observed in the analogous compound [Mendez-Rojas et al. (2001). J. Chem. Crystallogr. 31, 17–28] including a 2-oxo group [folding angle: 42.3 (1)° at 213 (2) K]. Both compounds are indeed isomorphous, and the small difference in the folding angle probably results from the involvement of the thioxo group of the title compound in inter­molecular S⋯S contacts [3.5761 (13) Å]. In the crystal structure, mol­ecules are stacked in the [100] direction, with dithiole rings making π–π inter­actions. In a stack, alternating short and long separations are observed between the centroids of dithiole rings, 3.5254 (17) and 4.7010 (18) Å. PMID:22219881

  11. Synthesis and structural study on (1E,2E,1'E,2'E)-3,3'-bis[(4-bromophenyl)-3,3'-(4-methy-1,2-phenylene diimine)] acetaldehyde dioxime: A combined experimental and theoretical study

    NASA Astrophysics Data System (ADS)

    Topal, T.; Kart, H. H.; Tunay Taşlı, P.; Karapınar, E.

    2015-06-01

    Tetradentate (1E,2E,1'E,2'E)-3,3'-bis[(4-bromophenyl)-3,3'-(4-methy-1,2-phenylene diimine)] acetaldehyde dioxime which possess N4 donor sets derived from the condensation of isonitroso- p-bromoacetophenone and 3,4-diaminotoluene are synthesized and characterized. The characterization of tetradentate Schiff base ligand has been deduced from LC-MS, FTIR, 13C and 1H NMR spectra and elemental analysis. Furthermore, the molecular geometry, infrared and NMR spectra of the title molecule in the ground state have been calculated by using the quantum chemical computational methods such as density functional theory (DFT) and ab initio Hartree-Fock (HF) methods with the 6-31G(d) and 6-311G(d) basis sets. The computed bond lengths and bond angles by using the both methods show the good agreement with each other. Moreover, the vibrational frequencies have been calculated and the scaled values have been compared with the experimental FTIR spectroscopic data. Assignments of the vibrational modes are made on the basis of potential energy distribution (PED) calculated from by using VEDA program. The correlations between the observed and calculated frequencies are in good agreement with each other as well as the correlation of the NMR data.

  12. 3-Acetyl-2-methyl-4-(pyridin-3-yl)-1,4-di­hydro­indeno­[1,2-b]pyridin-5-one

    PubMed Central

    Bisenieks, Imants; Mishnev, Anatoly; Bruvere, Imanta; Vigante, Brigita; Andzans, Zigmars

    2013-01-01

    In the title compound, C20H16N2O2, the condensed tricyclic fragment is near to planar, with an r.m.s. deviation of 0.0531 Å. The 1,4-di­hydro­pyridine (1,4-DHP) ring adopts a slightly puckered boat-like conformation. The N and opposite C atoms deviate from the least-squares plane of the four other ring atoms by 0.039 (3) and 0.141 (3) Å, respectively. The C=O group located at the tricyclic fragment is fixed in an s-trans orientation, while the second C=O group adopts an s-cis orientation with respect to the double bonds of the 1,4-DHP ring. The pyridine ring has a pseudo-axial orientation with respect to the 1,4-DHP ring. The dihedral angle between the tricyclic system and the pyridine ring is 77.3 (3)°. In the crystal, the pyridine N atom accepts a hydrogen bond from the N—H group of the 1,4-DHP ring. The hydrogen bonds link the mol­ecules into infinite C(8) chains along the b-axis direction. PMID:23723870

  13. MnO2/g-C3N4 nanocomposite with highly enhanced supercapacitor performance.

    PubMed

    Chang, Xueting; Zhai, Xinxin; Sun, Shibin; Gu, Danxia; Dong, Lihua; Yin, Yansheng; Zhu, Yanqiu

    2017-03-01

    A novel sandwich-like MnO2/g-C3N4 nanocomposite (NC) based on the integration of high-density MnO2 nanorods (NRs) onto the surfaces of two-dimensional (2D) g-C3N4 sheets has been successfully fabricated through a facile soft chemical route at low temperature. The MnO2/g-C3N4 NC electrode enhanced the supercapacitor (SC) performance, benchmarked against both the bare MnO2 NRs electrode and the MnO2/graphene oxide (GO) NC electrode, exhibiting high specific capacitance of 211 F/g at a current density of 1 A/g, with good rate capacity and cycling stability. The sandwich-like hybrid structure, the unique 2D structure of the g-C3N4 sheets and the presence of nitrogen in the g-C3N4 all contributed to the promising SC performance of the MnO2/g-C3N4 NC. This work demonstrated the advantages of the g-C3N4 sheets over the commonly-used GO sheets in the design of novel hybrid composite for enhanced capacitance performance of MnO2-based electrochemical SCs, and the results could be extended to other electrode materials for SCs.

  14. MnO2/g-C3N4 nanocomposite with highly enhanced supercapacitor performance

    NASA Astrophysics Data System (ADS)

    Chang, Xueting; Zhai, Xinxin; Sun, Shibin; Gu, Danxia; Dong, Lihua; Yin, Yansheng; Zhu, Yanqiu

    2017-03-01

    A novel sandwich-like MnO2/g-C3N4 nanocomposite (NC) based on the integration of high-density MnO2 nanorods (NRs) onto the surfaces of two-dimensional (2D) g-C3N4 sheets has been successfully fabricated through a facile soft chemical route at low temperature. The MnO2/g-C3N4 NC electrode enhanced the supercapacitor (SC) performance, benchmarked against both the bare MnO2 NRs electrode and the MnO2/graphene oxide (GO) NC electrode, exhibiting high specific capacitance of 211 F/g at a current density of 1 A/g, with good rate capacity and cycling stability. The sandwich-like hybrid structure, the unique 2D structure of the g-C3N4 sheets and the presence of nitrogen in the g-C3N4 all contributed to the promising SC performance of the MnO2/g-C3N4 NC. This work demonstrated the advantages of the g-C3N4 sheets over the commonly-used GO sheets in the design of novel hybrid composite for enhanced capacitance performance of MnO2-based electrochemical SCs, and the results could be extended to other electrode materials for SCs.

  15. Absolute Charge Exchange Cross Sections for ^3He^2+ Collisions with ^4He and H_2

    NASA Astrophysics Data System (ADS)

    Mawhorter, R. J.; Greenwood, J.; Smith, S. J.; Chutjian, A.

    2002-05-01

    The JPL charge exchange beam-line(J.B. Greenwood, et al., Phys. Rev A 63), 062707 (2001) was modified to increase the forward acceptance angle and enable the measurement of total charge-exchange cross sections for slow, light, highly-charged ion collisions with neutral targets(R. E. Olson and M. Kimura, J. Phys. B 15), 4231 (1982). Data are presented for single charge exchange cross sections for ^3He^2+ nuclei scattered by ^4He and H2 in the energy range 0.33-4.67 keV/amu. For both targets there is good agreement with Kusakabe, et al.(T. Kusakabe, et al., J. Phys. Soc. Japan 59), 1218 (1990). Angular collection is studied by a comparison with differential measurements(D. Bordenave-Montesquieu and R. Dagnac, J. Phys. B 27), 543 (1994), as well as with earlier JPL results(J.B. Greenwood, et al., Ap. J. 533), L175 (2000), ibid. 529, 605 (2000) using heavier projectiles and targets. This work was carried out at JPL/Caltech, and was supported through contract with NASA. RJM thanks the NRC for a Senior Associateship at JPL.

  16. The crystal structure of cesium biuranyl trisulphate, Cs2(UO2)2(SO4)3

    USGS Publications Warehouse

    Ross, M.; Evans, H.T.

    1960-01-01

    The crystal structure of the new compound Cs(UO2)2(SO4)3 has been determined by X-ray diffraction methods. The compound is tetragonal, space group P421m (D2d3), with a = 9??62 ?? 0??02, c = 8??13 ?? 0??01 A ??, and Z = 2; s.g. (calc.) = 4??80 ?? 0??03, s.g. (obs.) = 4??74 ?? 0??05. The compound forms plates parallel to (001) bounded by the form (110). Intensity data were obtained from Buerger precession photographs of the (hk0) and (0kl) reciprocal lattice nets. No corrections for absorption were made. The co-ordinates of the U and Cs atoms were obtained by interpretation of the Patterson projections normal to (001) and (100) and a plausible structure was derived from electron density projections. The final parameters of the structure were determined from subtraction electron density maps, least squares analysis of the structure factors, and spatial considerations. The compound has a layer structure consisting of (UO2)2(SO4)3]n2n- sheets paralle to (001), tied together by cesium ions. The UO22+ group is co-ordinated by five sulphate oxygens which form a nearly plane pentagon approximately normal to the uranyl axis. The Cs2 atom is co-ordinated by twelve oxygen atoms and the Cs1 atom by eight oxygen atoms. X-ray and optical data are also given for the compound Rb2UO2(SO4)2??2H2O. ?? 1960.

  17. Regulation of atypical MAP kinases ERK3 and ERK4 by the phosphatase DUSP2

    PubMed Central

    Perander, Maria; Al-Mahdi, Rania; Jensen, Thomas C.; Nunn, Jennifer A. L.; Kildalsen, Hanne; Johansen, Bjarne; Gabrielsen, Mads; Keyse, Stephen M.; Seternes, Ole-Morten

    2017-01-01

    The atypical MAP kinases ERK3 and ERK4 are activated by phosphorylation of a serine residue lying within the activation loop signature sequence S-E-G. However, the regulation of ERK3 and ERK4 phosphorylation and activity is poorly understood. Here we report that the inducible nuclear dual-specificity MAP kinase phosphatase (MKP) DUSP2, a known regulator of the ERK and p38 MAPKs, is unique amongst the MKP family in being able to bind to both ERK3 and ERK4. This interaction is mediated by a conserved common docking (CD) domain within the carboxyl-terminal domains of ERK3 and ERK4 and the conserved kinase interaction motif (KIM) located within the non-catalytic amino terminus of DUSP2. This interaction is direct and results in the dephosphorylation of ERK3 and ERK4 and the stabilization of DUSP2. In the case of ERK4 its ability to stabilize DUSP2 requires its kinase activity. Finally, we demonstrate that expression of DUSP2 inhibits ERK3 and ERK4-mediated activation of its downstream substrate MK5. We conclude that the activity of DUSP2 is not restricted to the classical MAPK pathways and that DUSP2 can also regulate the atypical ERK3/4-MK5 signalling pathway in mammalian cells. PMID:28252035

  18. Polarized spectral properties and potential application of large-size Nd3+:Ba3Gd2(BO3)4 crystal

    NASA Astrophysics Data System (ADS)

    Gao, S. F.; Lv, S. Z.; Zhu, Z. J.; Wang, Y.; You, Z. Y.; Li, J. F.; Xu, J. L.; Wang, H. Y.; Tu, C. Y.

    2014-06-01

    The Nd3+-doped Ba3Gd2(BO3)4 crystal with high optical quality and large size is reported in this paper. The growing processes and characteristics of Nd3+:Ba3Gd2(BO3)4 crystal are discussed. The absorption and luminescence spectra of Nd3+ in Ba3Gd2(BO3)4 crystal were measured at room temperature. The luminescence decay curve in correspondence with the 4F3/24I11/2 transition centered at 1062 nm was also measured. The JO intensity parameters Ωt (t = 2,4,6) were calculated to be Ω2 = 1.263, Ω4 = 2.496, Ω6 = 3.606. The radiative lifetime τr and fluorescence lifetime τf are 317.771 and 115 μs respectively, and the fluorescence quantum efficiency is 37.1%.

  19. VUV spectroscopy of complex fluoride systems Na0.4(Y1-xREx)0.6F2.2 (RE3+ = Nd3+, Tm3+)

    NASA Astrophysics Data System (ADS)

    Makhov, V. N.; Uvarova, T. V.; Kirm, M.; Vielhauer, S.

    2016-05-01

    Emission and excitation spectra as well as luminescence decay kinetics of complex non-stoichiometric fluoride crystals Na0.4(Y1-xNdx)0.6F2.2 (x = 0.005, 0.05, 0.2, 1) and Na0.4(Y1-xTmx)0.6F2.2 (x = 0.0005, 0.01, 0.05, 0.1) have been studied in the VUV spectral range at liquid-helium (T ∼ 10 K) temperatures. It has been shown that these crystals show intense broad-band VUV luminescence due to the interconfiguration 5d-4f transitions in Nd3+ and Tm3+ ions. Remarkable concentration quenching is observed for Nd3+ 5d-4f luminescence whereas fast (spin-allowed) 5d-4f luminescence of Tm3+ shows no concentration quenching for the studied doping level up to 10%. The spin-allowed 5d-4f luminescence of Tm3+ in these crystals was found to be rather weak compared to spin-forbidden 5d-4f luminescence because of efficient nonradiative relaxation from higher-energy 5d states of Tm3+ to the lowest-energy 5d level responsible for spin-forbidden 5d-4f luminescence. The studied fluoride systems can be considered as promising active media for the development of VUV solid state lasers with optical pumping.

  20. High-pressure Raman spectroscopic studies of hydrogarnet, katoite Ca3Al2(O4H4)3

    NASA Astrophysics Data System (ADS)

    Kato, M.; Kyono, A.

    2014-12-01

    We report in situ Raman spectroscopic studies of katoite in a diamond-anvil cell under hydrostatic conditions up to 10 GPa at room temperature. Two bands near 331 and 539 cm-1 are observed clearly at 1.1 GPa. In the cubic garnet structure, the lower frequency peak can be assigned to a mode of A1g + F2g symmetry and the higher frequency peak can be assigned to a mode with A1g + Eg + F2g symmetry. The band at 331 cm-1 in the A1g + F2g mode is assigned to O4H4-translational and librational motion and the band at 539 cm-1 in the A1g + Eg + F2g mode is assigned to OH-translational motion. The peak positions and shapes in the Raman spectra agree well with those measured under ambient conditions. With increasing pressure, the frequency of the F2g mode increases continuously with pressure derivative of 10 cm-1/GPa. Upon increasing pressure, the A1g + Eg + F2g modes split at 5 GPa and the intensity of the this Raman band gradually decrease due to the cubic-tetragonal phase transition. The most striking characteristic of the Raman spectrum of katoite is that compression leads to the extinction of the Raman-active mode derived from A1g + Eg + F2g symmetry.

  1. n-Propyl 2,3,4,6-tetra-O-acetyl-β-d-glucopyran-oside.

    PubMed

    Mönch, Bettina; Emmerling, Franziska; Kraus, Werner; Becker, Roland; Nehls, Irene

    2013-02-01

    THE TITLE COMPOUND [SYSTEMATIC NAME: (2R,3R,4S,5R,6R)-2-(acet-oxy-meth-yl)-6-propoxytetra-hydro-2H-pyran-3,4,5-triyl triacetate], C(17)H(26)O(10), was formed by a Koenigs-Knorr reaction of 2,3,4,6-tetra-O-acetyl-α-d-glucopyranosyl bromide and n-propanol. The central ring adopts a chair conformation. The crystal does not contain any significant inter-actions such as hydrogen bonds.

  2. Vanadium(V) tartrato complexes: speciation in the H3O+(OH-)/H2VO4-/(2R,3R)-tartrate system and X-ray crystal structures of Na4[V4O8(rac-tart)2].12H2O and (NEt4)4[V4O8((R,R)-tart)2].6H2O (tart = C4H2O6(4-)).

    PubMed

    Schwendt, Peter; Tracey, Alan S; Tatiersky, Jozef; Gáliková, Jana; Zák, Zdirad

    2007-05-14

    A study of the aqueous H3O+(OH-)/H2VO4-/(2R,3R)-tartrate system has been performed at 273 K in a 1.0 mol/L Na+(Cl-) ionic medium using 51V NMR spectroscopy. In this relatively complicated system, more than 12 different species were observed. Ligand concentration, vanadate concentration, and pH variation studies were carried out, particularly for the range of pH 5.8-8.0 and for pH 2.4. Chemical shifts, vanadium-ligand stoichiometry, and also composition and formation constants for some, but not all, species are given. Despite some reduction of vanadium(V) to vanadium(IV) in an acidic medium at pH approximately 2.4, the stoichiometries of the principal species in solution at this pH were determined. Electrospray ionization mass spectra for some solutions were obtained and were in accordance with the conclusions drawn from the speciation studies. A series of crystalline vanadium(V) tartrato complexes M4[V4O8(tart)2].aq were also prepared and characterized. X-ray diffraction studies of Na4[V4O8(rac-tart)2].12H2O (1) and (NEt4)4[V4O8((R,R)-tart)2].6H2O (2) revealed unique tetranuclear [V4O8(tart)2]4- ions for which the {V4O4} rings have boat conformations.

  3. A structural and electrochemical investigation of 1-alkyl-3-methylimidazolium salts of the nitratodioxouranate(VI) anions [[UO2(NO3)2]2(mu 4-C2O4)]2-, [UO2(NO3)3]-, and [UO2(NO3)4]2-.

    PubMed

    Bradley, Antonia E; Hardacre, Christopher; Nieuwenhuyzen, Mark; Pitner, William R; Sanders, David; Seddon, Kenneth R; Thied, Robert C

    2004-04-19

    The properties of the 1-butyl-3-methylimidazolium salt of the dinuclear mu(4)-(O,O,O',O'-ethane-1,2-dioato)bis[bis(nitrato-O,O)dioxouranate(VI)] anion have been investigated using electrochemistry, single-crystal X-ray crystallography, and extended X-ray absorbance fine structure spectroscopy: the anion structures from these last two techniques are in excellent agreement with each other. Electrochemical reduction of the complex leads to the a two-electron metal-centered reduction of U(VI) to U(IV), and the production of UO(2), or a complex containing UO(2). Under normal conditions, this leads to the coating of the electrode with a passivating film. The presence of volatile organic compounds in the ionic liquids 1-alkyl-3-methylimidazolium nitrate (where the 1-alkyl chain was methyl, ethyl, propyl, butyl, pentyl, hexyl, dodecyl, hexadecyl, or octadecyl) during the oxidative dissolution of uranium(IV) oxide led to the formation of a yellow precipitate. To understand the effect of the cation upon the composition and structure of the precipitates, 1-alkyl-3-methylimidazolium salts of a number of nitratodioxouranate(VI) complexes were synthesized and then analyzed using X-ray crystallography. It was demonstrated that the length of the 1-alkyl chain played an important role, not only in the composition of the complex salt, but also in the synthesis of dinuclear anions containing the bridging mu(4)-(O,O,O',O'-ethane-1,2-dioato), or oxalato, ligand, by protecting it from further oxidation.

  4. Variation in PTCHD2, CRISP3, NAP1L4, FSCB, and AP3B2 associated with spherical equivalent

    PubMed Central

    Chen, Fei; Duggal, Priya; Klein, Barbara E.K.; Lee, Kristine E.; Truitt, Barbara; Klein, Ronald; Iyengar, Sudha K.

    2016-01-01

    Purpose Ocular refraction is measured in spherical equivalent as the power of the external lens required to focus images on the retina. Myopia (nearsightedness) and hyperopia (farsightedness) are the most common refractive errors, and the leading causes of visual impairment and blindness in the world. The goal of this study is to identify rare and low-frequency variants that influence spherical equivalent. Methods We conducted variant-level and gene-level quantitative trait association analyses for mean spherical equivalent, using data from 1,560 individuals in the Beaver Dam Eye Study. Genotyping was conducted using the Illumina exome array. We analyzed 34,976 single nucleotide variants and 11,571 autosomal genes across the genome, using single-variant tests as well as gene-based tests. Results Spherical equivalent was significantly associated with five genes in gene-based analysis: PTCHD2 at 1p36.22 (p = 3.6 × 10−7), CRISP3 at 6p12.3 (p = 4.3 × 10−6), NAP1L4 at 11p15.5 (p = 3.6 × 10−6), FSCB at 14q21.2 (p = 1.5 × 10−7), and AP3B2 at 15q25.2 (p = 1.6 × 10−7). The variant-based tests identified evidence suggestive of association with two novel variants in linkage disequilibrium (pairwise r2 = 0.80) in the TCTE1 gene region at 6p21.1 (rs2297336, minor allele frequency (MAF) = 14.1%, β = –0.62 p = 3.7 × 10−6; rs324146, MAF = 16.9%, β = –0.55, p = 1.4 × 10−5). In addition to these novel findings, we successfully replicated a previously reported association with rs634990 near GJD2 at 15q14 (MAF = 47%, β = –0.29, p=1.8 × 10−3). We also found evidence of association with spherical equivalent on 2q37.1 in PRSS56 at rs1550094 (MAF = 31%, β = –0.33, p = 1.7 × 10−3), a region previously associated with myopia. Conclusions We identified several novel candidate genes that may play a role in the control of spherical equivalent. However, further studies are needed to replicate these findings. In addition, our results contribute to the

  5. Be(3)(AsO4)2.2H2O, a New Berylloarsenate Phase Containing ’Bridged’ Tetrahedral 3-Rings

    DTIC Science & Technology

    1993-02-15

    in a gold tube and heated to 5500ýC for 135 hours in a Leco TEMPRESTM bomb. Upon cooling, numerous needle- and shard -like crystals were recovered...in handlizg these materials. The structure of Be3 (AsOi) 2 .2H 2 0 was determined by standard single- crystal X-ray meth- ods (11). A suitable shard of...habit colorless shard crystal system monoclinic a (A) 16.318(2) b (A) 4.6664(3) C (A) 9.8755(7) C (0) 93.777(3) V (A3) 750.37 Z 4 space group C2/c

  6. Synthesis of β-NaYF4: Yb3+, Tm3+ @ TiO2 and β-NaYF4: Yb3+, Tm3+ @ TiO2 @ Au nanocomposites and effective upconversion-driven photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Duo, Shuwang; Zhang, JieJun; Zhang, Hao; Chen, Zhong; Zhong, Cuiping; Liu, Tingzhi

    2016-12-01

    The β-NaYF4: Yb3+, Tm3+ @ TiO2 nanocomposite has been prepared by a facile hydrothermal method followed by the hydrolysis of TBOT, and then NaYF4: Yb3+, Tm3+ @ TiO2, HAuCl4 and sodium citrate were put into an oil bath for reaction to obtain the β-NaYF4: Yb3+, Tm3+ @ TiO2 @ Au core-shell nanocomposite. XRD and HRTEM show that the samples exhibit the hexagonal phase NaYF4, anatase TiO2 and cubic Au, indicating that the core-shell phases of NaYF4-TiO2 or NaYF4-TiO2-Au coexist in these samples. EDS and XPS results show the presence of Na, Y, F, Ti, O and Au elements. When TiO2 was coated on the surface of upconversion nanomaterials of NaYF4: Yb3+, Tm3+, the photocatalytic activity was improved significantly, and the β-NaYF4: Yb3+, Tm3+ @ TiO2 nanocomposite gives the highest photodegradation efficiency for MB and RhB, and decomposes about 73% of MB or 80% of RhB within 4.5 h under simulated solar light irradiation respectively. When the ultraviolet light from simulated sunlight irradiation was removed by the addition of a UV filter, the β-NaYF4: Yb3+, Tm3+ @ TiO2 nanocomposite decomposes about 42% of MB or 48% of RhB within 4.5 h. It means that the upconversion-driven photocatalytic performance (decomposes 42% of MB or 48% of RhB) is more effective than UV light-driven photocatalytic performance (31% of MB or 32% of RhB) in the photodegradation process. In addition, the β-NaYF4: Yb3+, Tm3+ @ TiO2 @ Au core-shell nanocomposite does not exhibit the better photocatalytic activity, and the optimal research will be carried out in the future.

  7. RELAP5-3D Developmental Assessment: Comparison of Versions 4.0.3is and 2.4.2is

    SciTech Connect

    Paul D. Bayless

    2012-09-01

    Figures have been generated comparing the parameters used in the developmental assessment of the RELAP5-3D code using versions 4.0.3is and 2.4.2is. The figures, which are the same as those used in Volume III of the RELAP5-3D code manual, compare calculations using the semi-implicit solution scheme with available experiment data. These figures provide a quick, visual indication of how the code predictions changed between these two code versions and can be used to identify cases in which the assessment judgment may need to be changed in Volume III of the code manual. Changes to the assessment judgments made after reviewing all of the assessment cases are also provided.

  8. 40 CFR 35.935-4 - Step 2+3 projects.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 1 2011-07-01 2011-07-01 false Step 2+3 projects. 35.935-4 Section 35...+3 projects. A grantee which has received step 2=3 grant assistance must make submittals required by... preliminary plan of operation. The Regional Administrator shall give written approval of these...

  9. 40 CFR 35.935-4 - Step 2+3 projects.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 1 2010-07-01 2010-07-01 false Step 2+3 projects. 35.935-4 Section 35...+3 projects. A grantee which has received step 2=3 grant assistance must make submittals required by... preliminary plan of operation. The Regional Administrator shall give written approval of these...

  10. Synthesis and antitubercular activity of novel 4-substituted imidazolyl-2,6-dimethyl-N3,N5-bisaryl-1,4-dihydropyridine-3,5-dicarboxamides.

    PubMed

    Fassihi, Afshin; Azadpour, Zahra; Delbari, Neda; Saghaie, Lotfollah; Memarian, Hamid R; Sabet, Razieh; Alborzi, Abdolvahab; Miri, Ramin; Pourabbas, Bahman; Mardaneh, Jalal; Mousavi, Pegah; Moeinifard, Behzad; Sadeghi-Aliabadi, Hojjat

    2009-08-01

    A series of 4-substituted imidazolyl-2,6-dimethyl-N(3),N(5)-bisaryl-1,4-dihydropyridine-3,5-dicarboxamides were prepared. They were screened as antitubercular agents against Mycobacterium tuberculosis H(37)Rv. Minimum inhibitory concentrations (MICs) were determined using agar proportion method. Compound 3i with 1-benzyl-2-methylthio-1H-imidazole-5-yl substituent at C-4 position and 4'-chloromophenyl group at C-3 and C-5 positions of the 1,4-dihydropyridine ring was the most potent one among the tested compounds. It was as potent as rifampicin against M. tuberculosis H(37)RV. Compound 3l also was an active antitubercular agent with the same substituent as compound 3i at the C-4 position and 3'-pyridyl group at C-3 and C-5 positions of the 1,4-dihydropyridine ring.

  11. The crystal structure of 3-chloro-2-(4-methyl­phenyl)-2H-pyrazolo­[3,4-b]quinoline

    PubMed Central

    Sowmya, Haliwana B. V.; Suresha Kumara, Tholappanavara H.; Jasinski, Jerry P.; Millikan, Sean P.; Yathirajan, Hemmige S.; Glidewell, Christopher

    2015-01-01

    In the mol­ecule of 3-chloro-2-(4-methyl­phen­yl)-2H-pyrazolo­[3,4-b]quinoline, C17H12ClN3, (I), the dihedral angle between the planes of the pyrazole ring and the methyl­ated phenyl ring is 54.25 (9)°. The bond distances in the fused tricyclic system provide evidence for 10-π delocalization in the pyrazolo­pyridine portion of the mol­ecule, with diene character in the fused carbocyclic ring. In the crystal, mol­ecules of (I) are linked by two independent C—H⋯N hydrogen bonds, forming sheets containing centrosymmetric R 2 2(16) and R 6 4(28) rings, and these sheets are all linked together by π–π stacking inter­actions with a ring-centroid separation of 3.5891 (9) Å. PMID:25995882

  12. Anticolorectal cancer effects and pharmacokinetic application of 2, 2-Bis [4-(4-amino-3-hydroxyphenoxy) phenyl] adamantane

    PubMed Central

    Yang, Po-Sheng; Wang, Jane-Jen; Tsai, Tung-Hu; Wang, Yea-Hwey; Jan, Woan-Ching; Cheng, Shih-Ping; Chi, Chin-Wen; Hsu, Yi-Chiung

    2015-01-01

    2, 2-Bis (4-(4-amino-3-hydroxyphenoxy) phenyl) adamantane (DPA) induced growth inhibition in human cancer cells using the national cancer institute (NCI) anticancer drug screen. In our previous study, we demonstrated that DPA exerted growth inhibitory activities in the three human colon cancer cell lines (Colo 205, HT-29, and HCT-15). To identify the detailed mechanism, we examined the functional importance of p21 and p53 in DPA-induced anticancer effect. We used three isogenic colon cancer cell lines, HCT-116, HCT-116 p53-/-, and HCT-116 p21-/-, to evaluate the roles of p21 and p53 in the in vitro anticancer effects of DPA. DPA dose-dependently inhibited cell growth, cell migration and increased cell cycle at the G0/G1 phase in HCT116 cells but not in p21-/- and p53-/- isogenic HCT-116 cells. Additionally, Western blot showed that DPA treatment induced the p21, p53, and cyclin-E protein expressions in HCT-116 cells. The p21 associated cell cycle regulatory protein such as cyclin D, CDK4, and pRb were decreased after DPA treatment in HCT-116 cells. DPA decreased cell migration in HCT-116 and HCT-116 p53-/- but not in HCT-116 p21-/- cells. We observed the up-regulation of E-cadherin, p-p38, and p-Erk in DPA-treated HCT-116 group but not in HCT-116 p21-/- and HCT-116 p53-/- groups. We assumed that p21 was required for DPA-induced anti-colon cancer effect through the Erk and p38 pathway leading to cell cycle arrest and inhibition of cell motility. Mean (± SE) pharmacokinetic parameters of the DPA were as follows: AUC = 64.44 ± 8.41, Cmax = 1.56 ± 0.48 and t1/2 = 113.92 ± 58.19. The pharmacokinetic data suggest DPA can be applied to further clinical study. This is the first pharmacokinetic study of DPA, and indicated that anti-proliferation and the cell mobility inhibition effects of DPA in HCT116 WT cells may result from the induction of p21 through activation of ERK and p38 pathway. PMID:26628962

  13. (E)-4-(1,3-Benzodioxol-5-yl)but-3-en-2-one

    PubMed Central

    Sarveswari, S.; Vijayakumar, V.; Mathew, Priya Susan; Mendoza-Meroño, Rafael; García-Granda, Santiago

    2011-01-01

    In the title compound, C11H10O3, the benzodioxole ring adopts a flattened [puckering parameters: q 2 = 0.107 (2) Å, ϕ2 = 160 (1)°] envelope conformation with the methylene C atom as the flap. The crystal packing features chains, parallel to the c axis, composed of dimers connected by weak C—H–O hydrogen bonds and extending in layers in the bc plane. PMID:21522344

  14. (E)-1-(2,4-Dimethyl­quinolin-3-yl)-3-(4-methyl­phen­yl)prop-2-en-1-one

    PubMed Central

    Prasath, R.; Bhavana, P.; Butcher, Ray J.

    2012-01-01

    In the title compound, C21H19NO, there are two mol­ecules in the asymmetric unit (Z′ = 2). There are π–π inter­actions between these two mol­ecules [centroid–centroid distance = 3.678 (2) Å], as well as a weak C—H⋯O inter­action. The conformation adopted by the two mol­ecules is such that the quinoline mean plane and the benzene ring are almost perpendicular [89.04 (5) and 76.89 (4)°]. In each mol­ecule, the methyl group of the tolyl ring is disordered over two conformations, with occupancy ratios of 0.56 (3):0.44 (3) and 0.65 (3):0.35 (3). PMID:22590372

  15. Endosomal sorting of VAMP3 is regulated by PI4K2A.

    PubMed

    Jović, Marko; Kean, Michelle J; Dubankova, Anna; Boura, Evzen; Gingras, Anne-Claude; Brill, Julie A; Balla, Tamas

    2014-09-01

    Specificity of membrane fusion in vesicular trafficking is dependent on proper subcellular distribution of soluble N-ethylmaleimide-sensitive factor attachment protein receptors (SNAREs). Although SNARE complexes are fairly promiscuous in vitro, substantial specificity is achieved in cells owing to the spatial segregation and shielding of SNARE motifs prior to association with cognate Q-SNAREs. In this study, we identified phosphatidylinositol 4-kinase IIα (PI4K2A) as a binding partner of vesicle-associated membrane protein 3 (VAMP3), a small R-SNARE involved in recycling and retrograde transport, and found that the two proteins co-reside on tubulo-vesicular endosomes. PI4K2A knockdown inhibited VAMP3 trafficking to perinuclear membranes and impaired the rate of VAMP3-mediated recycling of the transferrin receptor. Moreover, depletion of PI4K2A significantly decreased association of VAMP3 with its cognate Q-SNARE Vti1a. Although binding of VAMP3 to PI4K2A did not require kinase activity, acute depletion of phosphatidylinositol 4-phosphate (PtdIns4P) on endosomes significantly delayed VAMP3 trafficking. Modulation of SNARE function by phospholipids had previously been proposed based on in vitro studies, and our study provides mechanistic evidence in support of these claims by identifying PI4K2A and PtdIns4P as regulators of an R-SNARE in intact cells.

  16. Oxa-ene reaction of enols of amides with 4-phenyl-1,2,4-triazoline-3,5-dione.

    PubMed

    Basheer, Ahmad; Rappoport, Zvi

    2008-01-04

    The reaction of 16 enols of amides with 4-phenyl-1,2,4-triazoline-1,3-dione gave open chain adducts rather than the [2 + 2] cycloadducts with a hemiaminal moiety, both in solid state and in solution. This assignment is based on X-ray crystallography, (1)H and (13)C NMR data, and IR spectra. The suggested mechanism involves hydroxyl proton loss in a formal oxa-ene reaction. Mechanistic details and a possible alternative are discussed.

  17. Synthesis and crystal structures of 7-bromo-5-(2‧-chloro)phenyl-3-hydroxy-1-methyl-1,2-dihydro-3H-1,4-benzodiazepin-2-one and 7-bromo-5-(2‧-chloro)phenyl-1-hexyl-1,2,4,5-tetrahydro-3H-1,4-benzodiazepin-2,3-dione

    NASA Astrophysics Data System (ADS)

    Kravtsov, Victor Ch.; Fonari, Marina S.; Gdaniec, Мaria; Pavlovsky, Victor I.; Andronati, Sergei A.; Semenishyna, Ekaterina A.

    2012-06-01

    Treatment of 7-bromo-5-(2'-chloro)phenyl-3-hydroxy-1,2-dihydro-3H-1,4-benzodiazepin-2-one (1) with methyl or hexyl tosylate resulted in 7-bromo-5-(2'-chloro)phenyl-3-hydroxy-1-methyl-1,2-dihydro-3H-1,4-benzodiazepin-2-one (2) and 7-bromo-5-(2'-chloro)phenyl-1-hexyl-1,2,4,5-tetrahydro-3H-1,4-benzodiazepin-2,3-dione (3). As confirmed by X-ray crystallography, the two products differ not only in the identity of the alkyl substituent in position 1 of the benzodiazepine fragment but also crystallize in different molecular forms resulting from proton migration. This alteration of the molecular structure leads to a significant change in the conformation of the central molecular fragment and influences the assembly mode in the crystal. In 3, centrosymmetric dimers formed via a pair of Nsbnd H⋯O hydrogen bonds are further linked into chains via Csbnd Br⋯Odbnd C halogen bond interaction. In turn in 2 there are two symmetry independent molecules, each giving a different set of intermolecular interactions. One of the molecules forms a dimer via Osbnd H⋯O interactions whereas the second one generates chain via Csbnd Br⋯Odbnd C halogen bond that is also assisted by a weak Osbnd H⋯Br hydrogen bond.

  18. 40 CFR 721.7280 - 1,3-Propanediamine, N,N′-1,2-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ...-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl...-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl-4..., reaction products with N-butyl-2,2,6,6-tetramethyl-4-piperidinamine (PMN P-89-632) is subject to...

  19. 40 CFR 721.7280 - 1,3-Propanediamine, N,N′-1,2-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl...-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl-4..., reaction products with N-butyl-2,2,6,6-tetramethyl-4-piperidinamine (PMN P-89-632) is subject to...

  20. 40 CFR 721.7280 - 1,3-Propanediamine, N,N′-1,2-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ...-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl...-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl-4..., reaction products with N-butyl-2,2,6,6-tetramethyl-4-piperidinamine (PMN P-89-632) is subject to...

  1. 40 CFR 721.7280 - 1,3-Propanediamine, N,N′-1,2-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ...-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl...-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl-4..., reaction products with N-butyl-2,2,6,6-tetramethyl-4-piperidinamine (PMN P-89-632) is subject to...

  2. 40 CFR 721.7280 - 1,3-Propanediamine, N,N′-1,2-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...-ethanediylbis-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl...-, polymer with 2,4,6-trichloro-1,3,5-triazine, reaction products with N-butyl-2,2,6,6-tetramethyl-4..., reaction products with N-butyl-2,2,6,6-tetramethyl-4-piperidinamine (PMN P-89-632) is subject to...

  3. YCa3(CrO)3(BO3)4: A Cr(3+) Kagomé Lattice Compound Showing No Magnetic Order down to 2 K.

    PubMed

    Wang, Chun-Hai; Avdeev, Maxim; Kennedy, Brendan J; Küpers, Michael; Ling, Chris D

    2016-08-01

    We report a new gaudefroyite-type compound YCa3(CrO)3(BO3)4, in which Cr(3+) ions (3d(3), S = 3/2) form an undistorted kagomé lattice. Using a flux agent, the synthesis was significantly accelerated with the typical calcining time reduced from more than 2 weeks to 2 d. The structure of YCa3(CrO)3(BO3)4 was determined by combined Rietveld refinements against X-ray and neutron diffraction data. Symmetry distortion refinement starting from a disordered YCa3(MnO)3(BO3)4 model was applied to avoid overparameterization. There are two ordering models, namely, K2-1 and K2-2, with the space groups P63 (No. 173) and P3̅ (No. 147), respectively, that differ in the [BO3] ordering between different channels (in-phase or out-of-phase). Both models give similarly good fits to the diffraction data. YCa3(CrO)3(BO3)4 is an insulator with the major band gap at Eg = 1.65 eV and a second transition at 1.78 eV. Magnetically, YCa3(CrO)3(BO3)4 is dominated by anti-ferromagnetic exchange along edge-sharing CrO6 octahedral chains perpendicular to the kagomé planes, with Θ ≈ -120 K and μeff ≈ 3.92 μB. The compound shows no spin ordering or freezing down to at least 2 K.

  4. N-[(2S)-2-(4-Bromo­phen­yl)-4-oxo-1,3-thia­zolidin-3-yl]pyridine-3-carboxamide

    PubMed Central

    Akkurt, Mehmet; Çelik, Ísmail; Demir, Hale; Özkırımlı, Sumru; Büyükgüngör, Orhan

    2010-01-01

    In the title compound, C15H12BrN3O2S, the dihedral angle between the pyridine and benzene rings is 73.17 (19)°. The five-membered 1,3-thia­zolidine ring has an envelope conformation, with the S atom displaced by 0.196 (1) Å from the mean plane of the four other ring atoms. An intra­molecular C—H⋯N inter­action occurs. The crystal structure is stabil­ized by inter­molecular N—H⋯O and C—H⋯O hydrogen bonds and C—H⋯π inter­actions. In addition, a weak π–π stacking inter­action is also observed between the 1,3-thia­zolidine and pyridine rings [centroid–centroid distance = 3.805 (2) Å]. PMID:21587914

  5. Unusual reaction paths of SN2 nucleophile substitution reactions CH4 + H- → CH4 + H- and CH4 + F- → CH3F + H-: Quantum chemical calculations

    NASA Astrophysics Data System (ADS)

    Minyaev, Ruslan M.; Quapp, Wolfgang; Schmidt, Benjamin; Getmanskii, Ilya V.; Koval, Vitaliy V.

    2013-11-01

    Quantum chemical (CCSD(full)/6-311++G(3df,3pd), CCSD(T)(full)/6-311++G(3df,3pd)) and density function theory (B3LYP/6-311++G(3df,3pd)) calculations were performed for the SN2 nucleophile substitution reactions CH4 + H- → CH4 + H- and CH4 + F- → CH3F + H-. The calculated gradient reaction pathways for both reactions have an unusual behavior. An unusual stationary point of index 2 lies on the gradient reaction path. Using Newton trajectories for the reaction path, we can detect VRI point at which the reaction path branches.

  6. (5R)-3-(2-Chloro­acet­yl)-4-methyl-5-phenyl-1,3,4-oxadiazinan-2-one

    PubMed Central

    Caracelli, Ignez; Coelho, Daniel C. S.; Olivato, Paulo R.; Rodrigues, Alessandro; Tiekink, Edward R. T.

    2011-01-01

    The 1,3,4-oxadiazinan-2-one ring in the title compound, C12H13ClN2O3, is in a distorted half-chair conformation. The phenyl and chloro­acetyl groups occupy axial and equatorial positions, respectively, and lie to the opposite side of the mol­ecule to the N-bound methyl substituent. Mol­ecules are consolidated in the crystal structure by C—H⋯O inter­actions. PMID:21836983

  7. Crystal structure of 3-amino-2-propyl­quinazolin-4(3H)-one

    PubMed Central

    El-Hiti, Gamal A.; Smith, Keith; Hegazy, Amany S.; Alanazi, Saud A.; Kariuki, Benson M.

    2015-01-01

    In the title mol­ecule, C11H13N3O, the propyl group is almost perpendicular to the quinazolin-4(3H)-one mean plane, making a dihedral angle of 88.98 (9)°. In the crystal, mol­ecules related by an inversion centre are paired via π–π overlap, indicated by the short distances of 3.616 (5) and 3.619 (5) Å between the centroids of the aromatic rings of neighbouring mol­ecules. Inter­molecular N—H⋯N and N—H⋯O hydrogen bonds form R 6 6(30) rings and C(5) chains, respectively, generating a three-dimensional network. Weak C—H⋯O inter­actions are also observed. PMID:26396813

  8. 40 CFR 721.8940 - Chromate(3-), bis[3-[[6-amino-1,4-dihydro-2-[[[4-[(2-hydroxy-1-naphthalenyl)azo] phenyl]sulfonyl...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...] amino]-4-(oxo-.kappa.O)-5- pyrimidinyl]azo-.kappaN1] -4-hydroxy-.kappa.O)-5-nitrobenzenesulfonato(3... Specific Chemical Substances § 721.8940 Chromate(3-), bis phenyl]sulfonyl] amino]-4-(oxo-.kappa.O)-5- pyrimidinyl]azo-.kappaN1] -4-hydroxy-.kappa.O)-5-nitrobenzenesulfonato(3-)]-, trisodium. (a)...

  9. 40 CFR 721.8940 - Chromate(3-), bis[3-[[6-amino-1,4-dihydro-2-[[[4-[(2-hydroxy-1-naphthalenyl)azo] phenyl]sulfonyl...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...] amino]-4-(oxo-.kappa.O)-5- pyrimidinyl]azo-.kappaN1] -4-hydroxy-.kappa.O)-5-nitrobenzenesulfonato(3... Specific Chemical Substances § 721.8940 Chromate(3-), bis phenyl]sulfonyl] amino]-4-(oxo-.kappa.O)-5- pyrimidinyl]azo-.kappaN1] -4-hydroxy-.kappa.O)-5-nitrobenzenesulfonato(3-)]-, trisodium. (a)...

  10. Synthesis of 1,4-, 2,4-, and 3,4-dimethylphenanthrenes: A novel deoxygenation of arene 1,4-endoxides with trimethylsilyl iodide

    SciTech Connect

    Jung, Keeyong; Koreeda, Masato )

    1989-11-24

    A mild, efficient synthesis of the carcinogen 1,4-dimethylphenanthrene (2) and its bay-region methyl-bearing regioisomers 2,4-dimethyl- and 3,4-dimethylphenanthrenes (3 and 4) is described. The synthesis involves a generally applicable strategy that features a furan/dimethyl-1-naphthyne cycloaddition reaction followed by a convenient direct deoxygenation of the resulting enooxide with excess trimethylsilyl iodide generated in situ. The Friedel-Crafts cyclization of p-xylene with {gamma}-butyrolactone/AlCl{sub 3} or {gamma}-(2,5-dimethylphenyl)butyric acid via its trifluoromethanesulfonic anhydride derivative results in the formation of a mixture of 5,8-, 6,8-, and 5,7-dimethyl-1-tetralones (17, 20, and 21, respectively) through migration of aromatic methyl groups. The precursor to 6,8-dimethyl-1-naphthyne (10) was prepared from tetralone 20, isolable only as a 5:1 inseparable mixture with 17 from the direct Friedel-Crafts cyclization of p-xylene with {gamma}-butyrolactone, by {alpha}-dibromination with CuBr{sub 2}, dehydrobromination, and tosylation. The precursors to 5,8-dimethyl-1-naphthyne (9) and 7,8-dimethyl-1-naphthyne (11) were synthesized from the corresponding 1-naphthols 15 and 31, respectively. The synthesis of these naphthols involved cycloaddition between the corresponding dimethylated benzyne and furan followed by acid-catalyzed isomerization.

  11. Synthesis of some new 1,2,4-triazole derivatives starting from 3-(4-chlorophenyl)-5-(4-methoxybenzyl)-4H-1,2,4-triazol with anti-lipase and anti-urease activities.

    PubMed

    Bekircan, Olcay; Menteşe, Emre; Ulker, Serdar; Kucuk, Cagatay

    2014-06-01

    In the present study, starting compound 4 was prepared by deamination of compound 2 in the presence of hypophosphorous acid and sodium nitrite. Treatment of compound 4 with ethyl bromoacetate produced ethyl[3-(4-chlorophenyl)-5-(4-methoxybenzyl)-4H-1,2,4-triazol-4-yl]acetate (5), which was converted to the hydrazide derivative (6) by treatment with hydrazine hydrate. The reaction of compound 6 with aromatic aldehydes resulted in the formation of arylidene hydrazides (7). Treatment of 6 with CS2 in the presence of potassium hydroxide (KOH), followed by cyclization with hydrazine hydrate, afforded 4-amino-5-{[3-(4-chlorophenyl)-5-(4-methoxybenzyl)-4H-1,2,4-triazol-4-yl]methyl}-2,4-dihydro-3H-1,2,4-triazole-3-thione (9). The condensation of 9 with appropriate aldehydes gave Schiff bases (10), which were converted into Mannich bases (11) in the presence of formaldehyde. All the synthesized compounds were screened for their anti-lipase and anti-urease activities. Compounds 7b, 7d, 11b, 11c, and 11d showed moderate-to-good lipase inhibitory effects compared to orlistat. Compounds 7b and 7d exhibited better anti-lipase activity. Furthermore, among the compounds tested, 11a and 11d were found to show high inhibitory effect against urease with IC50 values of 12.39 ± 0.35 and 16.12 ± 1.06 µg/mL, respectively. Compound 11c showed moderate inhibitory activity. The Mannich base containing compound 11 may be a source of good leads for the synthesis of lipase and urease dual inhibitors.

  12. Polarized spectroscopic properties of Er3+:BaGd2(MoO4)4 crystal

    NASA Astrophysics Data System (ADS)

    Pan, Y.; Gong, X. H.; Chen, Y. J.; Lin, Y. F.; Huang, J. H.; Luo, Z. D.; Huang, Y. D.

    2012-05-01

    An Er3+:BaGd2(MoO4)4 single crystal has been grown by the Czochralski method. The polarized absorption spectra, polarized fluorescence spectra, and fluorescence decay curves were measured. In the framework of Judd-Ofelt theory, intensity parameters, spontaneous emission probabilities, fluorescence branching ratios, and radiative lifetimes were calculated. Besides, green upconversion fluorescence was also observed.

  13. Synthesis and antimicrobial activities of novel 1,2,4-triazolo [3,4-a] phthalazine derivatives.

    PubMed

    Zhang, Qiu-Rong; Xue, Deng-Qi; He, Peng; Shao, Kun-Peng; Chen, Peng-Ju; Gu, Yi-Fei; Ren, Jing-Li; Shan, Li-Hong; Liu, Hong-Min

    2014-02-15

    A series of novel 1,2,4-triazolo [3,4-a] phthalazine derivatives were synthesized in five steps from a common precursor, phthalic anhydride. Most of synthesized phthalazine derivatives showed inhibitory activity against Staphylococcus aureus. One of phthalazine derivatives 5l showed inhibitory activity against all tested bacterial and fungal strains.

  14. Synthesis and theoretical studies of non‒covalent interactions within a newly synthesized chiral 1,2,4-triazolo[3,4-b][1,3,4]thiadiazine

    NASA Astrophysics Data System (ADS)

    Yunus, Uzma; Ahmed, Shahbaz; Chahkandi, Mohammad; Bhatti, Moazzam H.; Tahir, Muhammad Nawaz

    2017-02-01

    In this work the synthesis of a new compound formulated as C12H12N4OS, ((S)-1-(6-Phenyl-7H-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazin-3-yl)ethanol) (5) reported and theoretical studies of the non‒covalent interactions constructed the related crystalline network described. It has been characterized by IR, Mass, and 1H, 13C NMR spectroscopy and single crystal X‒ray diffraction analysis. The binding energy of the non‒covalent interactions constructing the network of 5 have been calculated by dispersion corrected density functional theory (DFT‒D). The optimization of the formed network using H‒bonding and π‒stacking revealed that 1‒D coordination chain has been composed of neutral monomeric compound. For this purpose, the independent smallest fragment (monomer) and subsequently the related network, including seven monomers, having all non‒covalent interactions have been optimized. The results demonstrate that hydrogen bonds, especially Osbnd H⋯N, Csbnd H⋯O, Csbnd H⋯N, and Csbnd H⋯S interactions, govern the network formation. The calculated results of electronic transition in agreement with the experiment ones show eleven major bands derived from σ → π, n → n/σ*/π* aromatic rings to hydroxyl, inter‒atomic of oxygen, and thiadiazine to phenyl ring charge transfer transitions.

  15. Synthesis and Pharmacological Evaluation of α4β2 Nicotinic Ligands with a 3-Fluoropyrrolidine Nucleus.

    PubMed

    Tamborini, Lucia; Pinto, Andrea; Ettari, Roberta; Gotti, Cecilia; Fasoli, Francesca; Conti, Paola; De Micheli, Carlo

    2015-06-01

    Nicotinic acetylcholine receptors (nAChRs) play an important role in many central nervous system disorders such as Alzheimer's and Parkinson's diseases, schizophrenia, and mood disorders. The α(4)β(2) subtype has emerged as an important target for the early diagnosis and amelioration of Alzheimer's disease symptoms. Herein we report a new class of α(4)β(2) receptor ligands characterized by a basic pyrrolidine nucleus, the basicity of which was properly decreased through the insertion of a fluorine atom at the 3-position, and a pyridine ring carrying at the 3-position substituents known to positively affect affinity and selectivity toward the α(4)β(2) subtype. Derivatives 3-(((2S,4R)-4-fluoropyrrolidin-2-yl)methoxy)-5-(phenylethynyl)pyridine (11) and 3-((4-fluorophenyl)ethynyl)-5-(((2S,4R)-4-fluoropyrrolidin-2-yl)methoxy)pyridine (12) were found to be the most promising ligands identified in this study, showing good affinity and selectivity for the α(4)β(2) subtype and physicochemical properties predictive of a relevant central nervous system penetration.

  16. Calculation of the total electron excitation cross section in the Born approximation using Slater wave functions for the Li (2s yields 2p), Li (2s yields 3p), Na (3s yields 4p), Mg (3p yields 4s), Ca (4s yields 4p) and K (4s yields 4p) excitations. M.S. Thesis

    NASA Technical Reports Server (NTRS)

    Simsic, P. L.

    1974-01-01

    Excitation of neutral atoms by inelastic scattering of incident electrons in gaseous nebulae were investigated using Slater Wave functions to describe the initial and final states of the atom. Total cross sections using the Born Approximation are calculated for: Li(2s yields 2p), Na(3s yields 4p), k(4s yields 4p). The intensity of emitted radiation from gaseous nebulae is also calculated, and Maxwell distribution is employed to average the kinetic energy of electrons.

  17. Design and synthesis of 4-[3,5-dioxo-11-oxa-4,9-diazatricyclo[5.3.1.0(2,6)]undec-4-yl]-2-trifluoromethyl-benzonitriles as androgen receptor antagonists.

    PubMed

    Xiao, Hai-Yun; Balog, Aaron; Attar, Ricardo M; Fairfax, David; Fleming, Linda B; Holst, Christian L; Martin, Gregory S; Rossiter, Lana M; Chen, Jing; Cvjic, Mary-Ellen; Dell-John, Janet; Geng, Jieping; Gottardis, Marco M; Han, Wen-Ching; Nation, Andrew; Obermeier, Mary; Rizzo, Cheryl A; Schweizer, Liang; Spires, Thomas; Shan, Weifang; Gavai, Ashvinikumar; Salvati, Mark E; Vite, Gregory

    2010-08-01

    A novel series of 4-[3,5-dioxo-11-oxa-4,9-diazatricyclo[5.3.1.0(2,6)]undec-4-yl]-2-trifluoromethyl-benzonitriles has been synthesized. The ability of these compounds to act as antagonists of the androgen receptor was investigated and several were found to have potent activity in vitro and in vivo.

  18. Letters to the Editor: Tunable BeAl2O4:Ti3+ laser

    NASA Astrophysics Data System (ADS)

    Alimpiev, A. I.; Bukin, G. V.; Matrosov, V. N.; Pestryakov, Efim V.; Solntsev, V. P.; Trunov, V. I.; Tsvetkov, E. G.; Chebotaev, V. P.

    1986-05-01

    A study was made of a tunable laser with a new active medium in the form of a chrysoberyl crystal activated with trivalent titanium ions (BeAl2O4:Ti3+). Lasing due to the 2E-2T2 electronic-vibrational transition in Ti3+ was observed in the wavelength range 0.7-0.9μ when the active medium was pumped by the second harmonic of a YAG:Nd3+ laser (0.5μ).

  19. Biotransformation of 2,2',5,5'-tetrachlorobiphenyl (PCB 52) and 3,3',4,4'-tetrachlorobiphenyl (PCB 77) by liver microsomes from four species of sea turtles.

    PubMed

    Richardson, Kristine L; Schlenk, Daniel

    2011-05-16

    The rates of oxidative metabolism of two tetrachlorobiphenyl congeners were determined in hepatic microsomes from four species of sea turtles, green (Chelonia mydas), olive ridley (Lepidochelys olivacea), loggerhead (Caretta caretta), and hawksbill (Eretmochelys imbricata). Hydroxylation of 3,3',4,4'-tetrachlorobiphenyl (PCB 77), an ortho-meta unsubstituted rodent cytochrome P450 (P450) 1A substrate PCB, was not observed in sea turtle microsomes. Sea turtle microsomes hydroxylated 2,2',5,5'-tetrachlorobiphenyl (PCB 52), a meta-para unsubstituted rodent P450 family 2 substrate PCB, at rates ranging from less than 0.5 to 53 pmol/min/mg protein. The P450 inhibitor ketoconazole inhibited hydroxylation of PCB 52, supporting the role of P450 catalysis. Sea turtle PCB 52 hydroxlyation rates strongly correlated with immunodetected P450 family 2-like and less so with P450 family 3-like hepatic proteins. Testosterone 6β-, 16α-, 16β-hydroxylase activities were also significantly correlated with the expression of these enzymes, indicating that P450 family 2 or P450 family 3 proteins are responsible for PCB hydroxylation in sea turtles. This study indicated species-specific PCB biotransformation in sea turtles and preferential elimination of meta-para unsubstituted PCB congeners over ortho-meta unsubstituted PCB congeners consistent with PCB accumulation patterns observed in tissues of sea turtles.

  20. DNA strand scission by the nephrotoxin [2,2'-bipyridine]-3,3',4,4'-tetrol-1,1'-dioxide and related compounds in the presence of iron.

    PubMed

    Cantin-Esnault, D; Oubrahim, H; Richard, J M

    2000-08-01

    The capacity of non-illuminated nephrotoxin orellanine ([2,2'-bipyridine]-3,3',4,4'-tetrol-1,1'-dioxide) to induce DNA damage in the presence of ferrous iron and dioxygen has been evaluated. Maximal single-strand breaks in plasmid DNA were obtained with a metal to ligand ratio 1:3. Instantaneous oxidation of Fe2+ in presence of orellanine under air was responsible for oxy-radical production concomitant to a stable ferric complex Fe(III)Or3 formation, leading to oxidative DNA breakage at physiological pH. DNA damage was lowered in the presence of SOD and catalase or DMSO, indicating a set of reactions that leads to oxy-radical generation. Iron chelators such as DTPA and EDTA had no protecting effect, Desferal slightly protected. GSH acted as an oxy-radical scavenger, whereas cysteine induced stronger damage. Closely related bipyridine compounds were also studied in presence of Fe2+ and O2 using a combination of spin-trapping and DNA-nicking experiments, none of which were able to chelate iron and induce damage at pH 7. Both catecholic moieties and aminoxide groups are required for observing breakage at physiological pH.

  1. Charge, orbital and spin ordering phenomena in the mixed valence manganite (NaMn3+(3))(Mn3+(2)Mn4+(2))O12.

    PubMed

    Prodi, A; Gilioli, E; Gauzzi, A; Licci, F; Marezio, M; Bolzoni, F; Huang, Q; Santoro, A; Lynn, J W

    2004-01-01

    Mixed-valence manganites with the ABO3 perovskite structure display a variety of magnetic and structural transitions, dramatic changes of electrical conductivity and magnetoresistance effects. The physical properties vary with the relative concentration of Mn3+ and Mn4+ in the octahedral corner-sharing network, and the proportion of these two cations is usually changed by doping the trivalent large A cation (for example, La3+) with divalent cations. As the dopant and the original cation have, in general, different sizes, and as they are distributed randomly in the structure, such systems are characterized by local distortions that make it difficult to obtain direct information about their crystallographic and physical properties. On the other hand, the double oxides of formula AA'3Mn4O12 contain a perovskite-like network of oxygen octahedra centred on the Mn cations, coupled with an ordered arrangement of the A and A' cations, whose valences control the proportion of Mn3+ and Mn4+ in the structure. The compound investigated in this work, (NaMn3+(3))(Mn3+(2)Mn4+(2))O12, contains an equal number of Mn3+ and Mn4+ in the octahedral sites. We show that the absence of disorder enables the unambiguous determination of symmetry, the direct observation of full, or nearly full, charge ordering of Mn3+ and Mn4+ in distinct crystallographic sites, and a nearly perfect orbital ordering of the Mn3+ octahedra.

  2. Charge, orbital and spin ordering phenomena in the mixed valence manganite (NaMn3+3)(Mn3+2Mn4+2)O12

    NASA Astrophysics Data System (ADS)

    Prodi, A.; Gilioli, E.; Gauzzi, A.; Licci, F.; Marezio, M.; Bolzoni, F.; Huang, Q.; Santoro, A.; Lynn, J. W.

    2004-01-01

    Mixed-valence manganites with the ABO3 perovskite structure display a variety of magnetic and structural transitions, dramatic changes of electrical conductivity and magnetoresistance effects. The physical properties vary with the relative concentration of Mn3+ and Mn4+ in the octahedral corner-sharing network, and the proportion of these two cations is usually changed by doping the trivalent large A cation (for example, La3+) with divalent cations. As the dopant and the original cation have, in general, different sizes, and as they are distributed randomly in the structure, such systems are characterized by local distortions that make it difficult to obtain direct information about their crystallographic and physical properties. On the other hand, the double oxides of formula AA'3Mn4O12 contain a perovskite-like network of oxygen octahedra centred on the Mn cations, coupled with an ordered arrangement of the A and A' cations, whose valences control the proportion of Mn3+ and Mn4+ in the structure. The compound investigated in this work, (NaMn3+3)(Mn3+2Mn4+2)O12, contains an equal number of Mn3+ and Mn4+ in the octahedral sites. We show that the absence of disorder enables the unambiguous determination of symmetry, the direct observation of full, or nearly full, charge ordering of Mn3+ and Mn4+ in distinct crystallographic sites, and a nearly perfect orbital ordering of the Mn3+ octahedra.

  3. Pristine soils mineralize 3-chlorobenzoate and 2,4-dichlorophenoxyacetate via different microbial populations.

    PubMed Central

    Fulthorpe, R R; Rhodes, A N; Tiedje, J M

    1996-01-01

    Biodegradation of two chlorinated aromatic compounds was found to be a common capability of the microorganisms found in the soils of undisturbed, pristine ecosystems. We used 2,4-dichlorophenoxyacetate (2,4-D) and 3-chlorobenzoate (3CBA) as enrichment substrates to compare populations of degrading bacteria from six different regions making up two ecosystems. We collected soil samples from four Mediterranean (California, central Chile, the Cape region of South Africa, and southwestern Australia) and two boreal (northern Saskatchewan and northwestern Russia) ecosystems that had no direct exposure to pesticides or to human disturbance. Between 96 and 120 samples from each of the six regions were incubated with 50 ppm of [U-14C]2,4-D or [U-14C]3CBA. Soils from all regions samples mineralized both 2,4-D and 3CBA, but 3CBA was mineralized without a lag period, while 2,4-D was generally not mineralized until the second week. 3CBA degradative capabilities were more evenly distributed spatially than those for 2,4-D. The degradative capabilities of the soils were readily transferred to fresh liquid medium. 3CBA degraders were easily isolated from most soils. We recovered 610 strains that could release carbon dioxide from ring-labeled 3CBA. Of these, 144 strains released chloride and degraded over 80% of 1 mM 3CBA in 3 weeks or less. In contrast, only five 2,4-D degraders could be isolated, although a variety of methods were used in an attempt to culture the degraders. The differences in the distribution and culturability of the bacteria responsible for 3CBA and 2,4-D degradation in these ecosystems suggest that the two substrates are degraded by different populations. We also describe a 14C-based microtiter plate method that allows efficient screening of a large number of samples for biodegradation activity. PMID:8919776

  4. 27 CFR 555.214 - Storage within types 1, 2, 3, and 4 magazines.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ..., 3, and 4 magazines. 555.214 Section 555.214 Alcohol, Tobacco Products, and Firearms BUREAU OF... Storage § 555.214 Storage within types 1, 2, 3, and 4 magazines. (a) Explosive materials within a magazine... materials are not to be unpacked or repacked inside a magazine or within 50 feet of a magazine, and must...

  5. Studies on three-dimensional coordination polymer [Cd2(N2H4)2(N3)4]n: crystal structure, thermal decomposition mechanism and explosive properties.

    PubMed

    Liu, Zhenhua; Zhang, Tonglai; Zhang, Jianguo; Wang, Shaozong

    2008-06-15

    A 3D coordination polymer of cadmium(II) hydrazine azide, [Cd2(N2H4)2(N3)4]n, was synthesized and characterized by elemental analysis and Fourier transform infrared (FT-IR) spectrum. Its crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to monoclinic, P2(1)/c space group, a=12.555(2)A, b=11.724(2)A, c=7.842(1)A, beta=94.56(2) degrees and Z=4. The crystal contains two crystallographically independent sets of distorted octahedral Cd(II) atoms and dimeric units of Cd2N2, Cd2(NNN)2, Cd2(NN)2 through double micro-1, 1 azide bridges, micro-1, 3 azide bridges and bidentate bridging hydrazine ligands, respectively, and thus generating a 3D network structure. The thermal decomposition mechanism of the complex was studied by using differential scanning calorimetry (DSC), thermogravimetry-derivative thermogravimetry (TG-DTG) and FT-IR techniques. Under nitrogen atmosphere with a heating rate of 10 degrees C/min, the thermal decomposition of the complex contained two intense exothermic decomposition processes in the range of 150-304 degrees C in the DSC curve, and the final decomposed residue at 500 degrees C was Cd. Sensitivity tests revealed that the title complex is very insensitive to external stimuli.

  6. Tetra­kis(μ2-5-methyl­pyrazine-2-carboxyl­ato)-1:2κ3 N 1,O:O;2:3κ3 O:N 1,O;1:2κ2 O:O′;3:4κ2 O:O′-octa­octyl-1κ2 C,2κ2 C,3κ2 C,4κ2 C-di-μ3-oxido-1:2:3κ3 O;1:3:4κ3 O-tetra­tin(IV)

    PubMed Central

    Gao, Zhongjun; Li, Fahui

    2009-01-01

    The title compound, [Sn4(C8H17)8O2(C6H5N2O2)4], is a tetra­nuclear SnIV complex, built up by inversion symmetry around the central Sn2O2 ring. The SnIV coordination geometries are distorted SnO3C2 trigonal-bipyramidal and distorted SnO4C2 octa­hedral. The three-coordinate μ3-oxido bridging O atom in the Sn2O2 ring is attached to three Sn atoms. All non-H atoms, with the exception of the Sn-bonded octyl groups, lie approximately on a non-crystallographic mirror plane. PMID:21578611

  7. Design and synthesis of N-(5-chloro-2,4-dihydroxybenzoyl)-(R)-1,2,3,4-tetrahydroisoquinoline-3-carboxamides as novel Hsp90 inhibitors.

    PubMed

    Liang, Chuanpeng; Hao, Huilin; Wu, Xingkang; Li, Zhenyu; Zhu, Jing; Lu, Chunhua; Shen, Yuemao

    2016-10-04

    Heat shock protein 90 (Hsp90) is an attractive chemotherapeutic target for antitumor drug development. Herein, we reported the design and synthesis of two series of novel N-(5-chloro-2,4-dihydroxybenzoyl)-1,2,3,4-tetrahydroisoquinoline-3- carboxamides as Hsp90 inhibitors using (S)-Tic (1,2,3,4-tetrahydroisoquinoline-3- carboxylic acid) (A1-13) and (R)-Tic (B1-13) as scaffold, respectively. Cellular thermal shift assay (CETSA) screening showed that compounds B1-13 with (R)-Tic scaffold exhibited potent ability to stabilize Hsp90α. Compound B7 showed not only the most potent ability to induce thermal stabilization of Hsp90α but also the strongest cytotoxicity. The IC50 values of B7 were 0.98 μM and 1.74 μM against the proliferation of human breast cancer MDA-MB-231 and human cervical cancer HeLa cell lines, respectively. Moreover, CETSA melt and ITDRFCETSA (isothermal dose-response fingerprint) curves confirmed that B7 bound to Hsp90α in 293T cells. Western blotting results indicated that B7 induced the degradation of Hsp90 clients CDK4, Her2, Cdc-2 and C-raf. In addition, docking and Molecular dynamics (MD) refinement of the B7-Hsp90 complex showed that the binding model of B7 to Hsp90 was similar with that of 8-benzyladenines. The overall properties warrant compound B7 a promising lead for the development of Hsp90 inhibitor antitumor drugs.

  8. Spectroscopic analysis of Pr^3+ (4f^2) absorption intensities in a plastic host (HEMA).

    NASA Astrophysics Data System (ADS)

    Stonestreet, David; Nash, Kelly; Dee, Doug; Yow, Raylon; Gruber, John; Sardar, Dhiraj

    2006-10-01

    A spectroscopic investigation has been performed on the Pr^3+ ions embedded in 2-hydroxyethyl methacrylate (HEMA) solid plastic host. The standard Judd-Ofelt analysis was applied to the room temperature absorption intensities of Pr^3+ transitions to determine three phenomenological intensity parameters: φ2, φ4 and φ6. Values of the intensity parameters were subsequently used to determine the decay rates (emission probabilities), radiative lifetimes, and branching ratios of the principal intermanifold transitions of Pr^3+ from the ^3P2, ^1D2, and ^3P0 manifold states to the lower-lying manifolds. The spectroscopic properties Pr^3+ in HEMA will be compared with those in glasses.

  9. INPP4B and PTEN Loss Leads to PI-3,4-P2 Accumulation and Inhibition of PI3K in TNBC.

    PubMed

    Reed, Darien E; Shokat, Kevan M

    2017-02-14

    Triple-negative breast cancer [TNBC, lacks expression of estrogen receptor (ER), progesterone receptor (PR) and amplification of HER2/Neu] remains one of the most aggressive subtypes, affects the youngest patients and still lacks an effective targeted therapy(1,2). Both phosphatidylinositol-3-kinase (PI3K)-α and -β contribute to oncogenesis of solid tumors, including the development of breast cancer(3). Inositol polyphosphate-4-phosphatase type II (INPP4B) catalyzes the removal of the 4'-phosphate of phosphatidylinositol-(3,4-bisphosphate (PI-3,4-P2) creating phosphatidylinositol-3-phosphate(4). There is debate concerning whether PI-3,4-P2 contributes to Akt and downstream effector activation with the known canonical signaling second messenger, phosphatidylinositol-(3,4,5)-trisphosphate (PIP3) (5-7). If PI-3,4-P2 is a positive effector, INPP4B would be a negative regulator of PI3K signaling and there is some evidence to support this(4,8). Utilizing phosphatase and tensin homolog deleted on chromosome ten (PTEN)-null triple-negative breast tumor cell lines, it was unexpectedly found that silencing INPP4B decreased basal phospho-Akt (pAkt) and cellular proliferation, and in most cases sensitized cells to PI3K-α and -β isoform-specific inhibitors. Conversely, overexpression of INPP4B desensitized cells to PI3K inhibitors in a phosphatase activity-dependent manner. In summary, the current investigation of INPP4B in PTEN-null TNBC suggests new mechanistic insight and the potential for targeted therapy for this aggressive subset of breast cancer.

  10. [Bis((2,4-dioxo-1,2,3,4-tetrahydroquinazolin-3-yl)alkyl)disulfane and 3-(mercaptoalkyl)quinazolin-2,4(1H,3H)-dione: synthesis by ring transformation and antiviral activity. 42. Heterocyclic azines with heteroatoms in the 1- and 3- positions].

    PubMed

    Gütschow, M; Tonew, E; Leistner, S

    1995-10-01

    Reaction of N-(sulfonyloxy)phtalimide derivatives 1, 2, with cystamine and homocystamine, respectively, affords bis[2,4-dioxol-1,2,3,4-tetra-hydroquinazolin-3-yl)alkyl] disulfanes [sequence: see text] 3, which could be reduced to 3-(mercaptoalkyl)quinazoline-2,4(1H,3H)-diones. 5. (3-(2-Mercaptoethyl)quinazoline-2,4(1H,3H)-dione (5a) was also obtained in a one-pot reaction from 1 or 2 and cysteamine. 2-Ethoxy-4H-3,1-benzoxazin-4-ones 4a-c were converted with cysteamine to 3-(mercaptoethyl)quinazoline-2,4-diones 5a-c by a new ringtransformation reaction. 3-(2-Mercaptoethyl)quinazoline-2,4(1H,3H)dione (5a) and the corresponding disulfane 3a were evaluated for antiviral activity in vitro. Compounds 3a and 5a showed significant antiviral activity against some DNA- and RNA-viruses (vaccinia-, herpes simplex virus type 1; influenza A virus) at concentrations that were nontoxic to the host cell cultures.

  11. Laser-spectroscopy measurement of the fine-structure splitting 2 3P1-2 3P2 of 4He

    NASA Astrophysics Data System (ADS)

    Feng, G.-P.; Zheng, X.; Sun, Y. R.; Hu, S.-M.

    2015-03-01

    Laser spectroscopy has been performed on a beam of neutral 4He atoms. By using transverse laser cooling and focusing, we are able to prepare a bright beam of atoms in the metastable state 2 3S1 deflected from the original effusive atomic beam. The initial state preparation is completed with optical pumping on the 2 3P1←2 3S1 transition at the wavelength of 1083 nm, followed by laser spectroscopy on the 2 3P1 ,22 3S1 transitions. The 2 3P1-2 3P2 fine-structure splitting is determined to be 2 291 177.69 ±0.36 kHz . The quantum interference effect is included in data extraction. This is the most precise laser spectroscopy measurement of the interval. Our result is in agreement with both the latest QED-based calculation and the most precise measurement conducted with microwave spectroscopy.

  12. 4-(3-Methoxyphenyl)-2,6-dimethylcyclohex-3-enecarboxylic acid

    SciTech Connect

    Xie, Songwen; Nusbaum, Dannette A.; Stein, Holly J.; Pink, Maren

    2012-03-15

    The racemic title compound, C{sub 16}H{sub 20}O{sub 3}, was synthesized to study the hydrogen-bonding interaction of the two enantiomers in the solid state. In the crystal structure, R and S pairs of the racemate are linked by pairs of intermolecular O-H...O hydrogen bonds, producing centrosymmetric R{sub 2}{sup 2}(8) rings.

  13. Structure and bonding in Yb4MgGe4: Yb2+/Yb3+ mixed-valency and charge separation.

    PubMed

    Tobash, Paul H; Bobev, Svilen

    2006-03-22

    Reported are the synthesis and the structural characterization of a new derivative of the RE5Tt4 family (RE = Rare-earth; Tt = Tetrel, = Si, Ge, i.e., group 14 element), Yb5-xMgxGe4 (x approximately 1). Crystal data for Yb4.04(1)Mg0.96(1)Ge4 at 23 degrees C: orthorhombic, space group Pnma (No. 62), Z = 4; a = 7.155(2) A, b = 14.769(5) A, c = 7.688(2) A; V = 812.5(4) A3. This phase is an example of a substitution of lanthanide metal (Yb) with a nonmagnetic element (Mg) within this structure type. Its structure can alternatively be described as an intergrowth of the hypothetical Yb2MgGe2, which features flat infinite [MgGe2]4- layers and the hypothetical YbGe with [Ge2]6- dimers. The flat [MgGe2]4- layers propagate in two dimensions (a and c), and they are offset by a distance of 1/4.a with respect to one another and are interspaced with layers of [Ge2]6- dimers and Yb cations filling the space between them. According to the structural and physical property data, Yb4MgGe4 is a heterogeneous mixed-valent compound, i.e. a system where one of the two symmetry-inequivalent Yb sites has atoms in closed-shell Yb2+ configuration, whereas the Yb3+ cations occupy a different crystallographic site.

  14. Exocyclic Deoxyadenosine Adducts of 1,2,3,4-Diepoxybutane: Synthesis, Structural Elucidation, and Mechanistic Studies

    PubMed Central

    Seneviratne, Uthpala; Antsypovich, Sergey; Goggin, Melissa; Dorr, Danae Quirk; Guza, Rebecca; Moser, Adam; Thompson, Carrie; York, Darrin M.; Tretyakova, Natalia

    2009-01-01

    1,2,3,4-Diepoxybutane (DEB)1 is considered the ultimate carcinogenic metabolite of 1,3-butadiene, an important industrial chemical and environmental pollutant present in urban air. Although it preferentially modifies guanine within DNA, DEB induces a large number of A → T transversions, suggesting that it forms strongly mispairing lesions at adenine nucleobases. We now report the discovery of three potentially mispairing exocyclic adenine lesions of DEB: N6,N6-(2,3-dihydroxybutan-1,4-diyl)-2′-deoxyadenosine (compound 2), 1,N6-(2-hydroxy-3-hydroxymethylpropan-1,3-diyl)-2′-deoxyadenosine (compound 3), and 1,N6-(1-hydroxymethyl-2-hydroxypropan-1,3-diyl)-2′-deoxyadenosine (compound 4). The structures and stereochemistry of the novel DEB-dA adducts were determined by a combination of UV and NMR spectroscopy, tandem mass spectrometry, and independent synthesis. We found that synthetic N6-(2-hydroxy-3,4-epoxybut-1-yl)-2′-deoxyadenosine (compound 1) representing the product of N6-adenine alkylation by DEB spontaneously cyclizes to form 3 under aqueous conditions or 2 under anhydrous conditions in the presence of organic base. Compound 3 can be interconverted with 4 by a reversible unimolecular pericyclic reaction favoring 4 as a more thermodynamically stable product. Both 3 and 4 are present in double stranded DNA treated with DEB in vitro and in liver DNA of laboratory mice exposed to 1,3-butadiene by inhalation. We propose that in DNA under physiological conditions, DEB alkylates the N-1 position of adenine in DNA to form N1-(2-hydroxy-3,4-epoxybut-1-yl)-adenine adducts, which undergo an SN2-type intramolecular nucleophilic substitution and rearrangement to give 3 (minor) and 4 (major). Formation of exocyclic DEB-adenine lesions following exposure to 1,3-butadiene provides a possible mechanism of mutagenesis at the A:T base pairs. PMID:19883087

  15. Crystal structure and IR spectroscopic study of (CN{sub 3}H{sub 6}){sub 2}[(UO{sub 2}){sub 2}(C{sub 2}O{sub 4})(CH{sub 3}COO){sub 4}

    SciTech Connect

    Serezhkina, L. B.; Peresypkina, E. V.; Neklyudova, N. A.; Virovets, A. V.; Serezhkin, V. N.

    2013-03-15

    Compound (CN{sub 3}H{sub 6}){sub 2}[(UO{sub 2}){sub 2}(C{sub 2}O{sub 4})(CH{sub 3}COO){sub 4}] is synthesized and characterized by IR spectroscopy and single-crystal X-ray diffraction [a = 8.5264(2) A, b = 13.8438(4) A, c = 10.7284(2) A, {beta} = 103.543(1) Degree-Sign , space group P2{sub 1}/n, Z = 2, and R = 0.0258]. The main structural units of the crystals are binuclear [(UO{sub 2}){sub 2}C{sub 2}O{sub 4}(CH{sub 3}COO){sub 4}]{sup 2-} groups, which belong to the A{sub 2}K{sup 02}B{sub 4}{sup 01} crystal chemical group of uranyl complexes (A = UO{sub 2}{sup 2+}, K{sup 02} = C{sub 2}O{sub 4}{sup 2-}, and B{sup 01} = CH{sub 3}COO{sup -}). The coordination polyhedron of the uranium atom is the UO{sub 8} hexagonal bipyramid with the oxygen atoms of the uranyl ion at the axial positions. Uranium-containing groups and guanidinium cations are connected by electrostatic interactions and by the hydrogen bond system, which involves hydrogen atoms of guanidinium cations and oxygen atoms of oxalate and acetate anions. The results of the spectroscopic study of the compound agree with the X-ray diffraction data.

  16. Synthesis and luminescent properties of novel BaGd2O4:Eu3+ scintillating phosphor.

    PubMed

    Sun, Xin-Yuan; Wang, Wen-Feng; Sun, Shou-Qiang; Lin, Liang-Wu; Li, De-Yi; Zhou, Ling-Ping

    2013-01-01

    BaGd2-x O4:xEu(3+) and Ba1-y Gd1.79-2y Eu0.21 Na3y O4 phosphors were synthesized at 1300°C in air by conventional solid-state reaction method. Phosphors were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence excitation (PLE) spectra, photoluminescence (PL) spectra and thermoluminescence (TL) spectra. Optimal PL intensity for BaGd2-x O4 :xEu(3+) and Ba1-y Gd1.79-2y Eu0.21 Na3y O4 phosphors at 276 nm excitation were found to be x = 0.24 and y = 0.125, respectively. The PL intensity of Eu(3+) emission could only be enhanced by 1.3 times with incorporation of Na(+) into the BaGd2 O4 host. Enhanced luminescence was attributed to the flux effect of Na(+) ions. However, when BaGd2 O4:Eu(3+) phosphors were codoped with Na(+) ions, the induced defects confirmed by TL spectra impaired the emission intensity of Eu(3+) ions.

  17. Effect of Si3N4 powder reactivity on the preparation of the Si2N2O-Al2O3 silicon aluminum oxynitride solid solution

    NASA Technical Reports Server (NTRS)

    Sekercioglu, I.; Wills, R. R.

    1979-01-01

    Dense high-purity silicon aluminum oxynitride was prepared by reactive hot-pressing of an Si3N4-Al2O3-SiO2 mixture. The formation of a single-phase material was found to be critically dependent on the Si3N4 powder in the starting mixture. It is suggested that evolution of a chlorine- and nitrogen-containing species may enhance the reactivity of Si3N4 in this reaction. Densities of O prime sialons are very similar to that of Si2N2O, the widely quoted value in the ceramics literature of 3.1 g/cu cm for the density of Si2N2O being incorrect.

  18. The enthalpies of formation of nesquehonite, MgCO3 * 3H2O, and hydromagnesite, 5MgO * 4CO2 * 5H2O

    USGS Publications Warehouse

    Hemingway, Bruce S.; Robie, Richard A.

    1973-01-01

    The enthalpies of formation, ΔH°f, of nesquehonite, MgCO3 * 3H2O, and hydromagnesite, 5MgO * 4CO2 * 5H2O, have been determined by HCl solution calorimetry. For the reaction MgO(c) + CO2(g) + 3H2O(l) = MgCO2 * 3H2O(c), the enthalpy change at 298.15 K is -29,781*40 cal mor' . For the reaction 5MgO(c) + 4CO2 + 5H2O = 5MgO * 4CO2 * 5H2O, the enthalpy change at 298.15 K is -120,310±120 cal. For MgCO3 * 3H2O the standard molar enthalpy and standard Gibbs free energy of formation, ΔH°f,298 and ΔG°f,298 are -472,576+110 and 412,040±120 cal. ΔH°f,298 and ΔG°f,298 for 5MgO * 4CO2 * 5H2O are -1,557,090±250 and -1,401,71 0±250 cal.

  19. Five new anthocyanins, ternatins A3, B4, B3, B2, and D2, from Clitoria ternatea flowers.

    PubMed

    Terahara, N; Oda, M; Matsui, T; Osajima, Y; Saito, N; Toki, K; Honda, T

    1996-02-01

    Five new ternatins 1-5 have been isolated from Clitoria ternatea flowers, and the structures have been determined by chemical and spectroscopic methods as delphinidin 3-malonylG having 3'-GCG-5'-GCG, 3'-GCG-5'-GC, 3'-GCGCG-5'-GC, 3'-GCGC-5'-GCG, and 3'-GCGC-5'-GC side chains, respectively, in which G is D-glucose and C is p-coumaric acid. Pigment 1 had symmetric 3',5'-side chains. Compounds 3 and 4 are structural isomers. These ternatins were shown to form an intramolecular stacking between the aglycon ring and the 3',5'-side chains in solution.

  20. Synthesis of 3-((2,4-dichlorophenoxy)methyl)-1,2,4-triazolo(thiadiazoles and thiadiazines) as anti-inflammatory and molluscicidal agents.

    PubMed

    El Shehry, M F; Abu-Hashem, A A; El-Telbani, E M

    2010-05-01

    A series of fused and non fused 1,2,4-triazoles with (2,4-dichlorophenoxy) moiety are prepared utilizing 3-((2,4-dichlorophenoxy)methyl)-4-amino-4H-1,2,4-triazole-5-thiol (3). The latter on reaction with carboxylic acids, ethylchloroformate, ethylcyanoacetate and sodium nitrite gives five membered fused triazole derivatives 4a-d, 5, 6, 7 and 10, respectively. The six membered heterocycles 11, 12 and 14 are prepared by cyclization of compound 3 with phenacyl bromide, chloroacetic acid and alpha-bromoketone respectively. Most of the newly synthesized compounds were screened for their anti-inflammatory and molluscicidal activities. The compounds 4b, 4d, 11 and 14 showed potent anti-inflammatory activities in dose dependent manner while compounds 3, 4b, 8 and 10 exhibited promising molluscicidal activities.

  1. 4,4-Dimethyl-2-[3-nitro-2-phenyl-1-(phenyl­sulfan­yl)prop­yl]-4,5-dihydro-1,3-oxazole

    PubMed Central

    Caracelli, Ignez; Zukerman-Schpector, Julio; Villar, José A. F. P.; Oliveira, Alfredo R. M.; Tiekink, Edward R. T.

    2012-01-01

    In the title compound, C20H22N2O3S, the oxazoline ring is planar (r.m.s. deviation = 0.045 Å) and forms dihedral angles of 47.24 (8) and 10.11 (8)° with the S- and C-bound phenyl rings, respectively. The nitro group lies to the same side of the mol­ecule as the oxazoline ring but is orientated so as not to inter­act with the ring. Linear supra­molecular chains along [010] are formed via C—H⋯O and C—H⋯S contacts. Chains are consolidated into a three-dimensional architecture by C—H⋯π and van der Waals inter­actions. PMID:22606161

  2. Synthesis and biological evaluation of 3,4-diphenyl-1,2,5-oxadiazole-2-oxides and 3,4-diphenyl-1,2,5-oxadiazoles as potential hybrid COX-2 inhibitor/nitric oxide donor agents.

    PubMed

    Velázquez, Carlos; Rao, P N Praveen; McDonald, Robert; Knaus, Edward E

    2005-04-15

    A group of 3,4-diphenyl-1,2,5-oxadiazole-2-oxides (3,4-diphenylfuroxans) and the corresponding N-desoxy 3,4-diphenyl-1,2,5-oxadiazoles (3,4-diphenylfurazans) analogs, were synthesized for in vitro evaluation as hybrid cyclooxygenase (COX) inhibitor/nitric oxide donor agents. Reaction of 1-[4-(methylsulfonyl)phenyl]-2-phenylethene with an aqueous sodium nitrite solution in acetic acid afforded a mixture (3:1 ratio) of the inseparable 4-[4-(methylsulfonyl)phenyl]-3-phenyl-1,2,5-oxadiazole-2-oxide (13a) and 3-[4-(methylsulfonyl)phenyl]-4-phenyl-1,2,5-oxadiazole-2-oxide (13b) regioisomers. A group of related regioisomers possessing either a p-aminosulfonylphenyl (16) or a p-azidosulfonylphenyl (17), moiety were obtained by chlorosulfonation of the unsubstituted 3,4-diphenylfuroxan (10) and subsequent reaction with either ammonium hydroxide or sodium azide, respectively. The methanesulfonyl regioisomers 13a,b [COX-1 IC50=11.6 microM; COX-2 IC50=0.12 microM; COX-2 selectivity index (SI)=97] and aminosulfonyl regioisomers 16 (COX-1 IC50=9.8 microM; COX-2 IC50=0.78 microM; COX-2 SI=12), like the reference drug celecoxib (COX-1 IC50=33.1 microM; COX-2 IC50=0.07 microM; COX-2 SI=472), were potent in vitro COX-2 inhibitors with a good COX-2 selectivity index. Release of nitric oxide (NO) from the 3,4-diphenylfuroxan compounds (10, 13a,b, 16, 17) was thiol-dependent since the % NO released was higher upon incubation in the presence of l-cysteine (0.57-3.18%) compared to that in phosphate buffer solution at pH7.4 (0.06-0.15%). Molecular modeling (docking) studies show that the methanesulfonyl (MeSO2) COX-2 pharmacophore present in regioisomers 13a,b is positioned in the vicinity of the COX-2 secondary pocket. The in vitro NO release data, COX-1/COX-2 inhibition and COX-2 SI structure-activity relationships acquired, and molecular modeling docking studies suggest that the 1,2,5-oxadiazole-2-oxide (furoxan) ring possesses beneficial features that should be present in a suitable

  3. Photocatalytic decomposition of N2O over TiO2/g-C3N4 photocatalysts heterojunction

    NASA Astrophysics Data System (ADS)

    Kočí, K.; Reli, M.; Troppová, I.; Šihor, M.; Kupková, J.; Kustrowski, P.; Praus, P.

    2017-02-01

    TiO2/g-C3N4 photocatalysts with the various TiO2/g-C3N4 weight ratios from 1:2 to 1:6 were fabricated by mechanical mixing in water suspension followed by calcination. Pure TiO2 was prepared by thermal hydrolysis and pure g-C3N4 was prepared from commercial melamine by thermal annealing at 620 °C. All the nanocomposites were characterized by X-ray powder diffraction, UV-vis diffuse reflectance spectroscopy, Raman spectroscopy, infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, photoelectrochemical measurements and nitrogen physisorption. The prepared mixtures along with pure TiO2 and g-C3N4 were tested for the photocatalytic decomposition of nitrous oxide under UVC (λ = 254 nm), UVA (λ = 365 nm) and Vis (λ > 400 nm) irradiation. The TiO2/g-C3N4 nanocomposites showed moderate improvement compared to pure g-C3N4 but pure TiO2 proved to be a better photocatalyst under UVC irradiation. However, under UVA irradiation conditions, the photocatalytic activity of TiO2/g-C3N4 (1:2) nanocomposite exhibited an increase compared to pure TiO2. Nevertheless, further increase of g-C3N4 amount leads/led to a decrease in reactivity. These results are suggesting the nanocomposite with the optimal weight ratio of TiO2 and g-C3N4 have shifted absorption edge energy towards longer wavelengths and decreased the recombination rate of charge carriers compared to pure g-C3N4. This is probably due to the generation of heterojunction on the TiO2/g-C3N4 interface.

  4. Redetermination of ruizite, Ca2Mn3+ 2[Si4O11(OH)2](OH)2·2H2O

    PubMed Central

    Fendrich, Kim V.; Downs, Robert T.; Origlieri, Marcus J.

    2016-01-01

    The crystal structure of ruizite, ideally Ca2Mn3+ 2[Si4O11(OH)2](OH)2·2H2O [dicalcium dimanganese(III) tetra­silicate tetra­hydroxide dihydrate] was first determined in space group A2 with an isotropic displacement parameter model (R = 5.6%) [Hawthorne (1984 ▸). Tschermaks Mineral. Petrogr. Mitt. 33, 135–146]. A subsequent refinement in space group C2/m with anisotropic displacement parameters for non-H atoms converged with R = 8.4% [Moore et al. (1985 ▸). Am. Mineral. 70, 171–181]. The current study reports a redetermination of the ruizite structure by means of single-crystal X-ray diffraction data of a natural sample from the Wessels mine, Kalahari Manganese Field, Northern Cape Province, South Africa. Our data (R 1 = 3.0%) confirm that the space group of ruizite is that of the first study rather than C2/m. This work improves upon the structure reported by Hawthorne (1984 ▸) in that all non-H atoms were refined with anisotropic displacement parameters and all hydrogen atoms were located. The crystal structure consists of [010] chains of edge-sharing MnO6 octa­hedra flanked by finite [Si4O11(OH)2] chains. The Ca2+ cations are situated in the cavities of this arrangement and exhibit a coordination number of seven. PMID:27555940

  5. 2-[(Z)-4,7-Dichloro-3,3-dimethyl-2,3-dihydro-1H-indol-2-yl-idene]-3-oxopropane-nitrile.

    PubMed

    Helliwell, Madeleine; Baradarani, Mehdi M; Mohammadnejadaghdam, Razieh; Afghan, Arash; Joule, John A

    2012-01-01

    In the title compound, C(13)H(10)Cl(2)N(2)O, the ring N atom and its three attached atoms are essentially coplanar with angles adding to 359.8°, indicating conjugation with the 2-formyl-acrylonitrile subunit. The aldehyde group is oriented to place the carbonyl O atom 2.02 (3) Å from the N-H hydrogen atom. Intra-molecular N-H⋯O and C-H⋯Cl inter-actions occur. The geometry of the exocyclic double bond is Z. In the crystal, weak C-H⋯N hydrogen bonds link the mol-ecules into chains along [1[Formula: see text]0].

  6. Highly regio- and stereocontrolled formation of functionalized tricyclo[4.2.1.0(2,8)]non-3-enes.

    PubMed

    Toselli, Nicolas; Martin, David; Achard, Mathieu; Tenaglia, Alphonse; Buono, Gérard

    2009-05-15

    The electrophilic activations of bicyclo[4.2.1]nonatrienes by 4-isopropyl-1,2,4-triazolinedione, N-iodosuccinimide, or an epoxidation/acidic ring-opening sequence is reported. The subsequent in situ trappings by water, alcohols, or benzoic acids led to original tricyclo[4.2.1.0(2,8)]non-3-enes with high regio- and stereoselectivities. The synthetic potentiality of these synthons is illustrated by the straightforward access to a fused cyclopropane featuring six consecutive controlled stereocenters.

  7. Reversible shuttle action upon dehydration and rehydration processes in cationic coordinatively-bonded (4,4) square-grid nets threaded by supramolecular bonded anions, {[Cu(II)(4,4'-bpy)2(H2O)][Cu(II)(2-pySO3)3](NO3)}·H2O.

    PubMed

    Jiang, Yi-Min; Yin, Zheng; He, Kun-Huan; Zeng, Ming-Hua; Kurmoo, Mohamedally

    2011-03-21

    {[Cu(II)(4,4'-bpy)(2)(H(2)O)][Cu(II)(2-pySO(3))(3)](NO(3))}·H(2)O, obtained serendipitously by the reaction of the constituents in water, consists of parallel coordinatively bonded cationic (4,4) corrugated square-grids polymer of {[Cu(II)(4,4'-bpy)(2)(H(2)O)](2+)}(n) threaded by π-π and H-bonded supramolecular chains of [Cu(II)(2-pySO(3))(3)](-) through the open squares. A single-crystal to single-crystal transformation takes place upon removal of the noncoordinated water by controlled heating. The resulting structure exhibits a rearrangement of the coordination of the copper atoms in the grids, where the Cu-H(2)O bond is elongated from 2.250(3) to 2.628(3) Å while the Cu-NO(3) is shortened from 3.122(3) to 2.796(1) Å. This process is reversible as demonstrated by the single crystal structure after rehydration with corresponding bond distances of 2.224(3) and 3.152(3) Å. Such a cooperative effect may be associated with the Jahn-Teller distortion of the copper(II) ion accompanying the shuttle action of the hydrogen-bonded water and nitrate moiety.

  8. Aquatic Toxicity of 3-Nitro-1,2,4-Triazol-5-One

    DTIC Science & Technology

    2009-09-01

    Ceriodaphnia dubia in a 7 day survival and reproduction assay and the unicellular green algae Selenastrum capricornutum in a 96 hr growth inhibition...Distilled Water 8 2.1.3 Analytical Methods 8 2.2 NTO Stability Testing 8 2.3 Ceriodaphnia 7 Day Survival and Reproduction Assay 8 2.4 Algal Growth...of each concentration were placed into amber crimper vials, capped, then stored under Ceriodaphnia 7 day Survival and Reproduction test conditions

  9. Preparation and studies of new crystals in the K3H(SO4)2-(NH4)3H(SO4)2-H2O system

    NASA Astrophysics Data System (ADS)

    Dmitricheva, E. V.; Makarova, I. P.; Grebenev, V. V.; Dolbinina, V. V.; Verin, I. A.

    2014-05-01

    To elucidate the effect of isomorphic substitution on the kinetics of phase transitions, single crystals of (K x (NH4)1- x ) m H n (SO4)( m + n)/2 · yH2O solid solutions are grown from the K3H(SO4)2-(NH4)3H(SO4)2-H2O system, whose end members are known to undergo superprotonic phase transitions of fundamentally different kinetics. The chemical composition of the single crystals grown is determined by energy dispersive X-ray microanalysis. The thermal and optical behavior of (K,NH4)9H7(SO4)8 · H2O single crystals is studied in the temperature range 295-420 K and the crystal structure at 295 K is determined. A comparison of the results of the studies with data for crystal K9H7(SO4)8 · H2O published earlier shows that the substitution of ammonium for potassium atoms lowers the temperature of the structural phase transition by 8 K.

  10. Emissions of N2O from tropical forest soils - Response to fertilization with NH4(+), NO3(-), and PO4(3-)

    NASA Technical Reports Server (NTRS)

    Keller, M.; Kaplan, W. A.; Wofsy, S. C.; Da Costa, Jose Maria

    1988-01-01

    Undisturbed oxisols in a central Amazon tropical forest were fertilized with ammonium, nitrate, or phosphate. Enhanced emissions of N2O were observed for all treatments within one day of fertilization, with the response NO3(-) much greater than NH4(+) much greater than PO4(3-). Approximately, 0.5 percent of applied NO3(-) was converted to N2O within two weeks after application, with less than 0.1 percent of the NH4(+) converted to N2O. These experiments reveal a potentially large source of N2O from microbial reduction of NO3(-) in the clay soils of Amazonia.

  11. 3d-Metal Doped into LiMn2O4 Thin Films

    SciTech Connect

    Bates, J.B.; Ueda, A.; Zuhr, R.A.

    1998-11-01

    3d-metal (Me) doped LiMn{sub 2}O{sub 4} thin films were deposited by rf magnetron sputtering of Li[Mn{sub 1.9}Me{sub 0.1}]O{sub 4} targets in Ar + N{sub 2} and Ar + O{sub 2} gas mixtures and annealed at 750{degrees}C in O{sub 2} for 1 h. From XRD measurements, the structure of the Me-doped thin film was dependent upon the element and the deposition conditions. The doping level of Me/Mn of cubic phase was less than 0.1 by EDX measurements. The Ti-LiMn{sub 2}O{sub 4} films exhibited a capacity close to theoretical for stoichiometric LiMn{sub 2}O{sub 4}. This improvement at 4 V comes at the expense of the capacity at 5 V. Cells with Ti-doped films exhibited the same low capacity fade as those with undoped LiMn{sub 2}O{sub 4} cathodes. Similar electrochemical changes were observed with the Cr- and Zn-LiMn{sub 2}O{sub 4} films. The discharge capacities above 4.5 V for the Ni-doped films were about equal to those below 4.5 V, and the thin-film cells could be cycled reversibility between 3.5 and 5.3 V.

  12. Diaquabis[mu-(R,R)-tartrato-kappa4O1,O2:O3,O4]dinickel(II) trihydrate.

    PubMed

    Scherb, Sandra; Näther, Christian; Bensch, Wolfgang

    2002-02-01

    In the crystal structure of the title compound, [Ni(2)(C(4)H(4)O(6))(2)(H(2)O)(2)].3H(2)O, two nickel cations, two tartrate anions and two water molecules form the dimeric complex. Each nickel cation is in a distorted octahedral environment composed of four O atoms of two crystallographically independent tartrate anions, one water molecule and one O atom of a symmetry-equivalent tartrate anion. The asymmetric unit contains three additional water molecules which are connected via hydrogen bonding.

  13. A 3D microporous covalent organic framework with exceedingly high C3H8/CH4 and C2 hydrocarbon/CH4 selectivity.

    PubMed

    Ma, Heping; Ren, Hao; Meng, Shuang; Yan, Zhuojun; Zhao, Huanyu; Sun, Fuxing; Zhu, Guangshan

    2013-10-28

    Here we present a new 3D microporous COF with a uniform pore size (0.64 nm). MCOF-1 exhibits high adsorption selectivity towards C3H8, C2H6 and C2H4 over CH4 owing to the pore size and preferential adsorption.

  14. Synthesis and Characterization of 1,4-Dihydro-3,1-Benzoxazines and 1,2,3,4-Tetrahydroquinazolines: An Unknown Structure Determination Experiment

    ERIC Educational Resources Information Center

    Bendorf, Holly D.; Vebrosky, Emily N.; Eck, Brian J.

    2016-01-01

    In this experiment for an upper-division course in organic structure determination, each student prepares an unknown compound and characterizes the product using multiple spectroscopic techniques. The unknowns, 2-aryl-substituted 1,4-dihydro-3,1-benzoxazines and 1,2,3,4-tetrahydroquinazolines, are prepared in a single step by the condensation of…

  15. Total facial selectivity of a D-erythrosyl aromatic imine in [4π + 2π] cycloadditions; synthesis of 2-alkylpolyol 1,2,3,4-tetrahydroquinolines.

    PubMed

    Ferreira, Juliana; Duarte, Vera C M; Noro, Jennifer; Gil Fortes, António; Alves, Maria J

    2016-03-14

    Different electron-rich dienophiles were combined with the imine obtained from 2,4-O-benzylidene-d-erythrose and p-anisidine furnishing enantiomerically pure tetrahydroquinolines, by inverse electron-demand [4π + 2π] cycloaddition. The imine was also reacted with 2-substituted electron-rich 1,3-butadienes giving the diastereomeric pure product, resulting from the normal electron demand cycloaddition. The facial selectivity of both processes is proposed on the basis of a 1,4-relationship between the hydroxyl group and the nitrogen atom in the chiral N-(p-methoxyphenyl)imine derivative.

  16. Crystal structure of 3-amino-2-ethyl­quinazolin-4(3H)-one

    PubMed Central

    El-Hiti, Gamal A.; Smith, Keith; Hegazy, Amany S.; Baashen, Mohammed; Kariuki, Benson M.

    2015-01-01

    The mol­ecule of the title compound, C10H11N3O, is planar, including the ethyl group, as indicated by the N—C—C—C torsion angle of 1.5 (2)°. In the crystal, inversion-related mol­ecules are stacked along the a axis. Mol­ecules are oriented head-to-tail and display π–π inter­actions with a centroid-to-centroid distance of 3.6664 (8) Å. N—H⋯O hydrogen bonds between mol­ecules generate a ‘step’ structure through formation of an R 2 2(10) ring. PMID:26396885

  17. 2-(4-Methyl­phen­yl)-2-oxoethyl 3-bromo­benzoate

    PubMed Central

    Khan, Imtiaz; Ibrar, Aliya; Korzański, Artur; Kubicki, Maciej

    2012-01-01

    The mol­ecule of the title compound, C16H13BrO3, is built of two approximately planar fragments, viz. 3-bromo­benzoate [maximum deviation = 0.055 (2) Å and 2-oxo-2-p-tolyl­ethyl [maximum deviation = 0.042 (2) Å], inclined by 46.51 (7)°. In the crystal, weak C—H⋯O hydrogen bonds and Br⋯Br contacts [3.6491 (7) Å] connect the mol­ecules into infinite layers parallel to (-221). PMID:23476275

  18. Synthesis, antitubercular, antifungal and antibacterial activities of 6-substituted phenyl-2-(3'-substituted phenyl pyridazin-6'-yl)-2,3,4,5-tetrahydropyridazin-3-one.

    PubMed

    Islam, Mojahidul; Siddiqui, Anees A; Rajesh, Ramadoss

    2008-01-01

    A series of 6-substituted phenyl-2-(3'-substituted phenyl pyridazin-6'-yl)-2,3,4,5-tetrahydropyridazin-3-ones has been synthesized. An appropriate aromatic hydrocarbon reacts with succinic anhydride in presence of AlCl3 to yield beta-aroyl propionic acid. The corresponding acid was cyclized with hydrazine hydrate to give 6-(substituted aryl)-2,3,4,5-tetrahydro-3-pyridazinone, which was heated on steam bath with phosphorus(V) oxychloride to yield 3-chloro 6-substituted phenyl pyridazine. This intermediate after reaction with hydrazine hydrate was converted into 3-hydrazino-6-substituted phenyl pyridazine. The resulting product was converted into 6-substituted phenyl-2-(3'-substituted phenyl pyridazin-6'-yl)-2,3,4,5-tetrahydropyridazin-3-one by reacting with substituted aroyl propionic acid. Spectral data (IR, NMR, mass spectra) confirmed the structures of the synthesized compounds. The synthesized compounds were investigated for their in vitro antitubercular, antifungal and antibacterial activities. The results indicated that the synthesized compounds have mild to potent activities with reference to their appropriate reference standards.

  19. Hydrothermal synthesis, crystal structure, conductivity, and thermal decomposition of [Cu(4,4'-bipy)(H2O)(Mo3O10)].H2O.

    PubMed

    Kong, Zuping; Weng, Linhong; Tan, Dejun; He, Heyong; Zhang, Biao; Kong, Jilie; Yue, Bin

    2004-09-06

    The hydrothermal reaction of (NH(4))(6)Mo(7)O(24).4H(2)O, CuCl(2).2H(2)O, and 4,4'-bipyridine yields bipyridine-ligated copper-trimolybdate monohydrate [Cu(4,4'-bipy)(H(2)O)(Mo(3)O(10))].H(2)O in the monoclinic system with space group of C(2/c) and cell parameters of a = 15.335(2) A, b = 15.535(2) A, c = 15.106(2) A, beta = 101.162(2) degrees, V = 3530.7(9) A(3), and Z = 8. Its structure consists of one-dimensional infinite ([Mo3O10]2-)( infinity ) chains linked through [Cu2(H2O)2(4,4'-bipy)] units. The Mo-O chain contains distorted [MoO(6)] octahedra connected through corner-sharing oxygen atoms into infinite chains along the c direction and each chain is located in the channel formed by four adjacent crossing chains of [Cu(4,4'-bipy)(H2O)](n)(2n+). The crystal shows weak conductivity through Mo-O chain along the c direction and insulating property along either a or b direction. Furthermore, a crystalline bimetallic oxide, CuMo3O10, forms when the title compound undergoes thermal treatment in N(2) atmosphere after the complete removal of the ligands.

  20. Raman spectroscopy of the multi-anion mineral schlossmacherite (H 3O,Ca)Al 3(AsO 4,PO 4,SO 4) 2(OH) 6

    NASA Astrophysics Data System (ADS)

    Frost, Ray L.; Palmer, Sara J.; Xi, Yunfei

    2012-02-01

    The mineral schlossmacherite (H 3O,Ca)Al 3(AsO 4,PO 4,SO 4) 2(OH) 6, a multi-cation-multi-anion mineral of the beudantite mineral subgroup has been characterised by Raman spectroscopy. The mineral and related minerals functions as a heavy metal collector and is often amorphous or poorly crystalline, such that XRD identification is difficult. The Raman spectra are dominated by an intense band at 864 cm -1, assigned to the symmetric stretching mode of the AsO 43- anion. Raman bands at 809 and 819 cm -1 are assigned to the antisymmetric stretching mode of AsO 43-. The sulphate anion is characterised by bands at 1000 cm -1 ( ν1), and at 1031, 1082 and 1139 cm -1 ( ν3). Two sets of bands in the OH stretching region are observed: firstly between 2800 and 3000 cm -1 with bands observed at 2850, 2868, 2918 cm -1 and secondly between 3300 and 3600 with bands observed at 3363, 3382, 3410, 3449 and 3537 cm -1. These bands enabled the calculation of hydrogen bond distances and show a wide range of H-bond distances.

  1. (2S,4E)-2-Hydroxy-4-octen-3-one, a Male-Produced Attractant Pheromone of the Cerambycid Beetle Tylonotus bimaculatus.

    PubMed

    Zou, Yunfan; Millar, Jocelyn G; Blackwood, J Scott; Van Duzor, Ryan; Hanks, Lawrence M; Mongold-Diers, Judith A; Wong, Joseph C H; Ray, Ann M

    2015-07-01

    We report the identification of a novel pheromone structure from males of the cerambycid beetle Tylonotus bimaculatus Haldeman (Cerambycinae: Hesperophanini), a species native to eastern North America. Volatiles collected from adult males contained (2S,4E)-2-hydroxyoct-4-en-3-one (71%), (3R,4E)-3-hydroxyoct-4-en-2-one (15%), (E)-4-octen-2,3-dione (13%), and 2,3-octanedione (1.5%). Four independent field bioassays with synthetic compounds confirmed that adults of both sexes were attracted by the racemate of the major component, (E)-2-hydroxyoct-4-en-3-one. No other cerambycid species were attracted in significant numbers. Attraction of both sexes is consistent with the male-produced pheromones of many other species in the subfamily Cerambycinae, but T. bimaculatus is unusual in having a pheromone chemistry that is so far unique among species in that subfamily.

  2. Crystal structure of 4-[(E)-(4-fluoro­benzyl­idene)amino]-3-methyl-1H-1,2,4-triazole-5(4H)-thione

    PubMed Central

    Manjula, P. S.; Sarojini, B. K.; Narayana, B.; Byrappa, K.; Madan Kumar, S.

    2015-01-01

    The title compound, C10H9FN4S, crystallizes with two mol­ecules (A and B) in the asymmetric unit. The dihedral angle between the planes of the trizole and fluoro­benzene rings is 7.3 (3)° in mol­ecule A and 41.1 (3)° in mol­ecule B. Mol­ecule A features an intra­molecular C—H⋯S hydrogen bond, which closes an S(6) ring. In the crystal, A+B dimers linked by pairs of N—H⋯S hydrogen bonds occur, generating R 2 2(8) loops. Weak π–π stacking contacts [centroid–centroid separation = 3.739 (6) Å] are also observed. PMID:26870523

  3. Bis(diethylenetriamine-kappa3N)nickel(II) 5-amino-1,3,4-thiadiazole-2-sulfonamidate chloride monohydrate.

    PubMed

    Liu-Gonzalez, M; Sanz-Ruiz, F; Chufán, E E; Pedregosa, J C; Borras-Tortonda, J

    2001-10-01

    In the X-ray crystal structure of the title complex, [Ni(C(4)H(13)N(3))(2)](C(2)H(3)N(4)O(2)S(2))Cl.H(2)O, the coordination polyhedron is composed of non-centrosymmetric [Ni(diethylenetriamine)(2)](2+) cations in which the triamine ligands coordinate to the metal centre as tridentate ligands in a facial position. The Ni(II) ions are linked to six N atoms in an octahedral arrangement, slightly compressed in one extreme. The sulfonamide behaves as a counter-ion instead of as a ligand. Important information about the deprotonated sulfonamide group conformation has been obtained.

  4. Inhibitors of hepatitis C virus NS3.4A protease. Part 3: P2 proline variants.

    PubMed

    Perni, Robert B; Farmer, Luc J; Cottrell, Kevin M; Court, John J; Courtney, Lawrence F; Deininger, David D; Gates, Cynthia A; Harbeson, Scott L; Kim, Joseph L; Lin, Chao; Lin, Kai; Luong, Yu-Ping; Maxwell, John P; Murcko, Mark A; Pitlik, Janos; Rao, B Govinda; Schairer, Wayne C; Tung, Roger D; Van Drie, John H; Wilson, Keith; Thomson, John A

    2004-04-19

    We recently described the identification of an optimized alpha-ketoamide warhead for our series of HCV NS3.4A inhibitors. We report herein a series of HCV protease inhibitors incorporating 3-alkyl-substituted prolines in P(2). These compounds show exceptional enzymatic and cellular potency given their relatively small size. The marked enhancement of activity of these 3-substituted proline derivatives relative to previously reported 4-hydroxyproline derivatives constitutes additional evidence for the importance of the S(2) binding pocket as the defining pharmacophore for inhibition of the NS3.4A enzyme.

  5. N-(2,3-Dihydro-1,4-benzodioxin-6-yl)-4-fluoro-benzene-sulfonamide.

    PubMed

    Mughal, Shumaila Younas; Khan, Islam Ullah; Harrison, William T A; Khan, Muneeb Hayat; Arshad, Muhammad Nadeem

    2012-08-01

    In the title compound, C(14)H(12)FNO(4)S, the dihedral angle between the aromatic rings is 50.26 (9)° and the C-S-N-C bond adopts a gauche conformation [torsion angle = -68.12 (15)°]. The dihydro-dioxine ring is disordered over two orientations, which both approximate to half-chairs, in a 0.880 (7):0.120 (7) ratio. In the crystal, N-H⋯O hydrogen bonds link the mol-ecules into C(4) chains propagating in [100]. Weak C-H⋯O and C-H⋯F inter-actions consolidate the packing.

  6. Crystal structure of 3-(3-oxo-2,3,4,4a,5,6-hexa-hydro-benzo[h]cinnolin-2-yl)propionic acid.

    PubMed

    Meneghetti, Fiorella; Masciocchi, Daniela; Gelain, Arianna; Villa, Stefania

    2014-10-01

    The asymmetric unit of the title compound, C15H16N2O3, contains two independent mol-ecules, which present a different conformation of the carb-oxy-lic acid side chain [C-C-C-OH torsion angles = 65.3 (7) and -170.1 (5)°]. In both mol-ecules, the di-hydro-pyridazinone ring adopts a geometry inter-mediate between a twisted-boat and a half-chair conformation, while the central six-membered ring is almost in a half-boat conformation. In the crystal, mol-ecules are linked by O-H⋯Ok (k = ketone) hydrogen bonds, generating [01-1] chains. Aromatic π-π stacking contacts between the benzene and the di-hydro-pyridazinone rings [centroid-centroid distance [3.879 (9) Å] are also observed.

  7. Poly[(μ3-hydrogenphosphato)(4H-1,2,4-triazole-κN 1)zinc

    PubMed Central

    Aitenneite, Hafid; El Bouari, Abdeslam; Sebti, Said; Saadi, Mohamed; El Ammari, Lahcen; Adil, Karim

    2012-01-01

    The asymmetric unit of the title compound, [Zn(HPO4)(C2H3N3)]n, contains one Zn2+ cation, one (HPO4)2− anion and a 1,2,4 triazole ligand. The Zn2+ cation is coordinated in a quite regular tetra­hedral geometry by O atoms from three phosphate groups and a tertiary N atom from the triazole ring. Each phosphate anion is connected to three ZnII cations, leading to a series of corrugated organic–inorganic layers parallel to the ac plane. The overall structure involves stacking of complex hybrid organic–inorganic layers along the b axis. Cohesion in the crystal is ensured by an infinite three-dimensional network of N—H⋯O and O—H⋯O hydrogen bonds between the phosphate groups and the triazole ligands. PMID:23284388

  8. 2. 3/4 view looking SW showing threeroll can mill, reduction ...

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

    2. 3/4 view looking SW showing three-roll can mill, reduction gear, flywheel with steam engine in background. - Hacienda Azucarera la Igualdad, Sugar Mill Ruins & Steam Engine, PR Route 332, Guanica, Guanica Municipio, PR

  9. 40 CFR 721.8950 - Chromate(3-), bis[3-[[6-amino-1,4-dihydro-2-[[[4-[(2-hydroxy-1-naphthalenyl)azo] phenyl]sulfonyl...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...]amino]-4-(oxo-.kappa.O)-5-pyrimidinyl]azo-.kappaN1]-4-hydroxy-.kappa.O)-5-nitrobenzenesulfonato(3...-(oxo-.kappa.O)-5-pyrimidinyl]azo-.kappaN1]-4-hydroxy-.kappa.O)-5-nitrobenzenesulfonato(3-)]-, sodium... substance identified as chromate(3-), bis...

  10. 40 CFR 721.8950 - Chromate(3-), bis[3-[[6-amino-1,4-dihydro-2-[[[4-[(2-hydroxy-1-naphthalenyl)azo] phenyl]sulfonyl...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...]amino]-4-(oxo-.kappa.O)-5-pyrimidinyl]azo-.kappaN1]-4-hydroxy-.kappa.O)-5-nitrobenzenesulfonato(3...-(oxo-.kappa.O)-5-pyrimidinyl]azo-.kappaN1]-4-hydroxy-.kappa.O)-5-nitrobenzenesulfonato(3-)]-, sodium... substance identified as chromate(3-), bis...

  11. Production of 2,3-butanediol by a low-acid producing Klebsiella oxytoca NBRF4.

    PubMed

    Han, Sung-Hyuk; Lee, Jung-Eun; Park, Kyungmoon; Park, Yong-Cheol

    2013-01-25

    2,3-Butanediol (2,3-BDO) is a value-added chemical with great potential for the industrial production of synthetic rubber, plastic and solvent. For microbial production of 2,3-BDO, in this study, Klebsiella oxytoca NBRF4 was constructed by chemical mutation and screening against NaBr, NaBrO(3) and fluoroacetate. Among metabolic enzymes involved in the production of lactate, acetate and 2,3-BDO, K. oxytoca NBRF4 possessed 1.2 times lower specific activities of lactate dehydrogenase and phosphotransacetylase, and 22% higher specific acetoin reductase activity than the K. oxytoca ATCC43863 control strain. A series of batch fermentations in a defined medium and application of a statistical tool of response surface method led to the determination of optimal culture conditions: 10% dissolved oxygen level, pH 4.3 and 38°C. The actual results of batch fermentation at the optimal conditions using 44 g/L glucose were coincident with the predetermined values: 14.4 g/L 2,3-BDO concentration, 0.32 g/g yield. To increase 2,3-BDO titer, fed-batch fermentation of K. oxytoca NBRF4 was performed by an intermittent feeding of 800 g/L glucose to control its concentration around 5-20 g/L in the culture broth. Finally, 34.2g/L 2,3-BDO concentration and 0.35 g/g yield were obtained without organic acid production in 70 hours of the fed-batch culture, which were 2.4 and 1.2 times higher than those of the batch fermentation using 44 g/L glucose.

  12. Synthesis of 1,4-Benzodiazepine-2,5-diones by Base Promoted Ring Expansion of 3-Aminoquinoline-2,4-diones.

    PubMed

    Křemen, Filip; Gazvoda, Martin; Kafka, Stanislav; Proisl, Karel; Srholcová, Anna; Klásek, Antonín; Urankar, Damijana; Košmrlj, Janez

    2017-01-06

    An unprecedented reactivity of 3-aminoquinoline-2,4-diones is reported. Under basic conditions, these compounds undergo molecular rearrangement to furnish 1,4-benzodiazepine-2,5-diones. The transformations take place under mild reaction conditions by using 1,1,3,3-tetramethylguanidine, NaOEt, or benzyltrimethylammonium hydroxide as a base. A proposed mechanism of the rearrangement and the conformational equilibrium of 1,4-benzodiazepine-2,5-dione rings are discussed.

  13. Synthesis and evaluation of 3-[(2,4-dioxo-1,3,8-triazaspiro[4.6]undec-3-yl)methyl]benzonitrile derivatives as potential anticonvulsants.

    PubMed

    Madaiah, Malavalli; Prashanth, Maralekere K; Revanasiddappa, Hosakere D; Veeresh, Bantal

    2013-03-01

    New 3-[(2,4-dioxo-1,3,8-triazaspiro[4.6]undec-3-yl)methyl]benzonitrile derivatives 8-37 were synthesized and their pharmacological activities were determined with the objective to better understand their structure-activity relationship (SAR) for anticonvulsant activity. All the compounds were evaluated for their possible anticonvulsant activity by maximal electroshock seizure (MES) and pentylenetetrazole (PTZ) test. Compounds 11, 18, 31, and 32 showed significant and protective effect on seizure, when compared with the standard drug valproate. The same compounds were found to exhibit advanced anticonvulsant activity as well as lower neurotoxicity than the reference drug. From this study, it is quite apparent that there are at least three parameters for the activity of anticonvulsant drugs, that is, a lipophilic domain, a hydrophobic center, and a two-electron donor.

  14. Optically stimulated luminescence (OSL) response of Al2O3:C, BaFCl:Eu and K2Ca2(SO4)3:Eu phosphors.

    PubMed

    Kumar, Pratik; Bahl, Shaila; Sahare, P D; Kumar, Surender; Singh, Manveer

    2015-12-01

    This paper investigates the optically stimulated luminescence (OSL) response of BaFCl:Eu and K2Ca2(SO4)3:Eu phosphors for different doses and bleaching durations. The results have also been compared with the commercially available Landauer Al2O3:C (Luxel®) dosemeter. Nanocrystalline K2Ca2(SO4)3:Eu is known to be a sensitive thermoluminescent phosphor, but its OSL response is hardly reported. At first, pellets of nanocrystalline K2Ca2(SO4)3:Eu powder were prepared by adding Teflon as a binder. Their OSL signal was compared with that of the material in pure form, i.e. without adding the binder (in 100:1 ratio). It was observed that adding the binder does not appreciably affect the OSL intensity. On comparison with the commercially available Al2O3:C from Landauer, it was found that K2Ca2(SO4)3:Eu is around 15 times less sensitive than Al2O3:C. 'Homemade' BaFCl:Eu phosphor has also been studied. The intensity of BaFCl:Eu was ∼20 times more than the standard Al2O3:C dosemeter and ∼200 times more sensitive than K2Ca2(SO4)3:Eu in the dose range of 13-200 cGy. OSL dosemeters are believed to give luminescence signal even if they are read before, i.e. multiple reading may be possible under suitable conditions after single exposure. This was also checked for all the prepared dosemeters and it was found that Al2O3:C showed the least decrease of <2 %, followed by BaFCl:Eu of 15 % and K2Ca2(SO4)3:Eu with 20 %. Finally, Al2O3:C and BaFCl:Eu phosphors were also studied for their optical bleaching durations to which the respective signals get completely removed so that the phosphor can be re-used. It was observed that BaFCl:Eu is bleached faster and more easily than Al2O3:C.

  15. Enantioseparation, absolute configuration determination, and anticonvulsant activity of (+/-)-1-(4-aminophenyl)-7,8-methylenedioxy-1,2,3,5-tetrahydro-4H-2,3-benzodiazepin-4-one.

    PubMed

    Calabrò, Maria Luisa; Raneri, Daniela; Ficarra, Paola; Ferreri, Guido; De Sarro, Giovambattista; Bruno, Giuseppe; Zappalà, Maria; Micale, Nicola; Grasso, Silvana

    2007-01-01

    The resolution of 1-(4-aminophenyl)-7,8-methylenedioxy-1,2,3,5-tetrahydro-4H-benzodiazepin-4-one (+/-)-(R,S)-2 was accomplished by chiral HPLC. The absolute configuration of (+)-2, determined by X-ray crystallographic analysis, was R. The in vivo anticonvulsant activity of the enantiomers (+)-(R)-2 and (-)-(S)-2 is reported. It has been also demonstrated that compound (+/-)-(R,S)-2 in vivo undergoes oxidative metabolism to derivative 1.

  16. Two lead(II) 2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate complexes exhibiting different topologies and fluorescent properties

    NASA Astrophysics Data System (ADS)

    Chen, Zilu; Yan, Jiehua; Xing, Huihui; Zhang, Zhong; Liang, Fupei

    2011-05-01

    The reactions of PbCl 2 with 2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylic acid (H 3iso) gave two complexes [Pb(H 2iso) 2(H 2O)] n ( 1) and [Pb(Hiso)(H 2O)] n ( 2), which were characterized by IR spectroscopy, elemental analysis, thermogravimetric analysis, powder X-ray diffraction and single crystal X-ray diffraction analysis. The two complexes display different topologies. 1 shows a three-dimensional framework with the Schläfli symbol (4.8 5)(4.8 2) no matter if the weak Pb-O bonds are included or not. However, 2 presents a 3,3-connected two-dimensional sheet with the Schläfli symbol (4.8 2)(4.8 2) based on the calculation of only the normal Pb-O bonds and a 5,5-connected 3D network with the Schläfli symbol (4 15.6 4)(4 4.6 8.8 2) when the weak Pb-O bonds are also included. The fluorescent studies reveal an emission attributed to intraligand emission for 1 and an emission assigned to LMCT for 2.

  17. Lanthanide complexes of 3-acetyl-4-hydroxy-6-methyl-2H-pyran-2-one

    SciTech Connect

    Sitran, S; Fregona, D. ); Faraglia, G. )

    1990-01-01

    The title ligand (H(Dh), dehydroacetic acid) reacts with lanthanide(III) acetates in anhydrous methanol to form complexes of formula (M(Dh){sub 3}(MeOH)). When hydrated lanthanide acetates are used, hydrated compounds such as (Ce(Dh){sub 3}(H{sub 2}O)) or (Eu(Dh){sub 3}(H{sub 2}O)).H{sub 2}O are obtained. The reaction of lanthanum triacetate with H(Dh) yields the mixed complex (La(Dh){sub 2}(O{sub 2}CMe)), formation of the 1:3 complex also being unfavored in the presence of a large ligand excess. The complexes have been characterized by infrared and NMR ({sup 1}H and {sup 13}C) spectroscopy and by thermogravimetric measurements.

  18. Nuclear Emulsion Measurements of the Astronauts’ Radiation Exposures on Skylab Missions 2, 3 and 4,

    DTIC Science & Technology

    1975-12-10

    AD-AO19 804 NUCLEAR EMULSION MEASUREMENTS OF THE ASTRONAUTS’ RADIATION EXPOSURES ON SKYLAB MISSIONS 2, 3 AND 4 Hermann J. Schaefer, et al Naval...N/A NUCLEAR EMULSION MEASUREMENTS OF THE ASTRONAUTS’ RADIATION EXPOSURES ON SKYLAB MISSIONS 2, 3, AND 4. N/ ___ _ _ ANZ Hermann J. Schaefer and...corresponding shield distribution of the entire vehicle tesi alirections ofetionable whether the very large effort involved in this eask isd• ~~really

  19. Combustion Synthesis of Ca3(PO4)2 Net-Shape Surgical Implants

    NASA Technical Reports Server (NTRS)

    Ayers, Reed A.; Castillo, Martin; Gottoli, Guglielmo; Moore, John J.; Simske, Steven J.

    2006-01-01

    Self-propagating high-temperature combustion synthesis (SHS) is the basis of a method of making components of porous tricalcium phosphate [Ca3(PO4)2] and related compounds in net sizes and shapes for use as surgical implants that are compatible with bone. The SHS method offers advantages over prior methods of manufacturing Ca3(PO4)2-based surgical implants.

  20. Low-Quantum-Defect Solid State Lasers: 2-, 3-, or 4-Level

    DTIC Science & Technology

    2010-08-01

    IPG Photonics develop the world’s first 10 kW single-mode production fiber laser [6]. Another...Low-Quantum-Defect Solid State Lasers : 2-, 3 -, or 4-level? by Jeffrey O. White ARL-RP-0298 August 2010 A...Research Laboratory Adelphi, MD 20783-1197 ARL-RP-0298 August 2010 Low-Quantum-Defect Solid State Lasers : 2-, 3 -, or 4-level? Jeffrey