3H-1,2-Benzodithiole-3-thione

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Khaled Boukebbous

2016-10-01

Full Text Available The almost planar (r.m.s. deviation = 0.034 Å title compound, C7H4S3, was synthesized by reacting 2,2-dithiodibenzoic acid with phosphorus pentasulfide in xylene solution. In the crystal, short S...S [3.3727 (14, 3.3765 (13 and 3.4284 (13 Å] contacts and aromatic π–π stacking [shortest centroid–centroid separation = 3.618 (2 Å] are observed.

1,5-Dimethyl-4-(1-methyl-3-oxo-3-phenylprop-1-enylamino-2-phenyl-1H-pyrazol-3(2H-one

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Hualing Zhu

2011-07-01

Full Text Available In the title compound, C21H21N3O2, an intramolecular N—H...O interaction generates an S(6 ring, which stablizes the enamine–keto tautomer. The S(6 ring makes dihedral angles of 33.07 (7, 56.50 (8 and 38.59 (8°, respectively, with the benzoylacetone benzene ring and the antipyrine pyrazole and benzene rings.

(Carbonyl-1κC)bis-[2,3(η)-cyclo-penta-dien-yl][μ(3)-(S-methyl trithio-carbonato)methylidyne-1:2:3κC,S'':C:C](triphenyl-phosphine-1κP)(μ(3)-sulfido-1:2:3κS)dicobalt(II)iron(II) trifluoro-methane-sulfonate.

Science.gov (United States)

Manning, Anthony R; McAdam, C John; Palmer, Anthony J; Simpson, Jim

2008-04-10

The asymmetric unit of the title compound, [FeCo(2)(C(5)H(5))(2)(C(3)H(3)S(3))S(C(18)H(15)P)(CO)]CF(3)SO(3), consists of a triangular irondicobalt cluster cation and a trifluoro-methane-sulfonate anion. In the cation, the FeCo(2) triangle is symmetrically capped on one face by an S atom and on the other by a C atom linked to a methyl trithio-carbonate residue that bridges the Fe-C bond. Each Co atom carries a cyclo-penta-dienyl ligand while the Fe atom coordinates to one carbonyl and one triphenyl-phosphine ligand. In the crystal structure, the cation is linked to the anion by a number of weak non-classical C-H⋯O and C-H⋯F hydrogen bonds and weak S⋯O (3.317 Å) and S⋯F (3.198 Å) inter-actions. The structure is further stabilized by additional inter-molecular C-H⋯O, C-H⋯F and O⋯O (2.942 Å) contacts, together with an unusual S⋯π(Cp) inter-action (S⋯centroid distance = 3.385 Å), generating an extended network.

(E)-3-Hydr?oxy-13-methyl-16-[4-(methyl?sulfan?yl)benzyl?idene]-7,8,9,11,12,13,15,16-octa?hydro-6H-cyclo?penta?[a]phen?an????thren-17(14H)-one

OpenAIRE

Gunasekaran, B.; Murugan, R.; Narayanan, S. Sriman; Manivannan, V.

2008-01-01

In the title compound, C26H28O2S, the dihedral angles between the mean plane of the five membered ring and the 4-(methylsulfanyl)benzylidine ring in the two crystallographically independent molecules are 34.05 (10) and 40.53 (15)°. The packing is stabilized by intermolecular O—H...O and C—H...O interactions.

Experiences with liquid scintillation counting of 3H, 14C and 35S from plant material

International Nuclear Information System (INIS)

Das, S.K.

1974-01-01

Relative merits of different methods in radioassay of three soft beta emitting isotopes like 3 H, 14 C and 35 S from plant material have been assessed. The methods used are: (1) combustion method (2) use of tissue solubilizing agents and (3) wet digestion method. Results show that determinations of 14 C by combustion method; 3 H by combustion and Mahin and Lofberg's method; and 35 S by wet digestion method are superior for plant material than the other methods tried. (author)

7-Chloro-11a-phenyl-2,3,5,10,11,11a-hexahydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11-dione

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Vahan Martirosyan

2008-03-01

Full Text Available The title compound, C18H15ClN2O2, is a potential human immunodeficiency virus type-1 (HIV-1 non-nucleoside reverse transcriptase inhibitor. The pyrrolidine ring adopts an envelope and the diazepine ring a boat conformation. In the crystal structure, two isomers (R and S form centrosymmetric dimers via N—H...O hydrogen bonds.

Novel 2D or 3D alkaline-earth metal sulfonate-phosphonates based on [O 3S-C 2H 4-PO 3H] 2- ligand

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Du, Zi-Yi; Wen, He-Rui; Xie, Yong-Rong

2008-11-01

Three novel alkaline-earth metal sulfonate-phosphonates based on [O 3S-C 2H 4-PO 3H] 2- ligand, namely, [Ca(O 3SC 2H 4PO 3H)(H 2O) 2] ( 1), [Sr(O 3SC 2H 4PO 3H)] ( 2) and [Ba 2(O 3SC 2H 4PO 3H) 2] ( 3), have been synthesized by hydrothermal reactions. They represent the first structurally characterized alkaline-earth metal complexes of phosphonic acid attached with a sulfonate group. The structure of compound 1 features a 2D layer based on 1D chains of [Ca 2(PO 3) 2] bridged by -CH 2-CH 2-SO 3- groups. Compounds 2 and 3 show pillar-layer architecture based on two different inorganic layers linked by -CH 2-CH 2- groups. The inorganic layer in compound 2 features a 1D chain of edge-sharing SrO 8 polyhedra whereas that in compound 3 features an edge-sharing Ba 2O 14 di-polyhedral unit which is further corner-shared with four neighboring ones. The [O 3S-C 2H 4-PO 3H] 2- ligand shows diverse coordination modes in the three alkaline-earth metal sulfonate-phosphonates.

1,4-Dihydroxyquinoxaline-2,3(1H,4H-dione

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Wolfgang Frey

2008-03-01

Full Text Available The asymmetric unit of the title compound, C8H6N2O4, contains one half-molecule; a twofold rotation axis bisects the molecule. The quinoxaline ring is planar, which can be attributed to electron delocalization. In the crystal structure, intermolecular O—H...O hydrogen bonds link the molecules into R22(10 motifs, leading to layers, which interact via phenyl–phenyl interactions (C...C distances in the range 3.238–3.521 Å.

Catalyst-Dependent Chemoselective Formal Insertion of Diazo Compounds into C-C or C-H Bonds of 1,3-Dicarbonyl Compounds.

Science.gov (United States)

Liu, Zhaohong; Sivaguru, Paramasivam; Zanoni, Giuseppe; Anderson, Edward A; Bi, Xihe

2018-05-08

A catalyst-dependent chemoselective one-carbon insertion of diazo compounds into the C-C or C-H bonds of 1,3-dicarbonyl species is reported. In the presence of silver(I) triflate, diazo insertion into the C(=O)-C bond of the 1,3-dicarbonyl substrate leads to a 1,4-dicarbonyl product containing an all-carbon α-quaternary center. This reaction constitutes the first example of an insertion of diazo-derived carbenoids into acyclic C-C bonds. When instead scandium(III) triflate was applied as the catalyst, the reaction pathway switched to formal C-H insertion, affording 2-alkylated 1,3-dicarbonyl products. Different reaction pathways are proposed to account for this powerful catalyst-dependent chemoselectivity. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

(3R,6S,7aS-3-Phenyl-6-(phenylsulfanylperhydropyrrolo[1,2-c]oxazol-5-one

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Anthony D. Woolhouse

2009-05-01

Full Text Available Molecules of the title compound [systematic name: (2R,5S,7S-2-phenyl-7-phenylsulfanyl-1-aza-3-oxabicyclo[3.3.0]octan-8-one], C18H17NO2S, form high quality crystals even though they are only packed using C—H...O(carbonyl and weak C—H...S interactions. The dihedral angle between the aromatic rings is 85.53 (5°. The fused rings adopt envelope and twist conformations.

3-(2-Fluorophenylsulfinyl-2,5,7-trimethyl-1-benzofuran

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Hong Dae Choi

2013-06-01

Full Text Available In the title compound, C17H15FO2S, the benzofuran ring system, being essentially planar, with an r.m.s. deviation from the least-squares plane of 0.009 (2 Å, makes a dihedral angle of 79.02 (5° with the plane of the 2-fluorophenyl group. In the crystal, molecules are linked by pairs of weak C—H...O hydrogen bonds into centrosymmetric dimers.

Efficient method of enzymatic synthesis of nucleosides labelled with 14C and 3H

International Nuclear Information System (INIS)

Nejedly, Z.; Filip, J.

1988-01-01

The method is presented of enzymatic synthesis of nucleosides labelled with 14 C or 3 H either uniformly or specifically in the base or the deoxyribosyl or ribosyl moiety. The method is based on the ribosylation or deoxyribosylation of the nucleic acid bases (non-labelled or labelled with 14 C or 3 H) by the catalytic effect of enzymes occurring in the supernatant fractions of non-purified homogenates of Escherichia coli B. bacteria. The non-labelled and labelled nucleosides are used as donors of ribosyl or deoxyribosyl groups. The HPLC method is used for separating labelled nucleosides. The radiochemical purity of the labelled nucleosides is higher than 98%, molar activity ranges from 9.2 to 18.5 GBq.mmol -1 ( 14 C-labelled compounds) and from 0.6 to 1.9 TBq.mmol -1 (3H-labelled compounds). (author). 4 figs., 8 refs

6-Chloro-7-fluoro-4-oxo-4H-chromene-3-carbaldehyde

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Yoshinobu Ishikawa

2014-07-01

Full Text Available In the title compound, C10H4ClFO3, a chlorinated and fluorinated 3-formylchromone derivative, all atoms are essentially coplanar (r.m.s. = 0.0336 Å for the non-H atoms, with the largest deviation from the least-squares plane [0.062 (2 Å] being for a benzene-ring C atom. In the crystal, molecules are linked through stacking interactions [centroid–centroid distance between the benzene and pyran rings = 3.958 (3 Å and interplanar distance = 3.259 (3 Å], C—H...O hydrogen bonds, and short C...O contacts [2.879 (3 Å]. Unsymmetrical halogen–halogen interactions between the Cl and F atoms [Cl...F = 3.049 (3 Å, C—Cl...F = 148.10 (9° and C—F...Cl = 162.06 (13°] are also formed, giving a meandering two-dimensional network along the a axis.

2-Methylsulfanyl-5,6-dihydro-2H-1,3-dithiolo[4,5-b][1,4]dioxin-2-ium tetrafluoroborate

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Guoquan Zhou

2012-04-01

Full Text Available The title compound, C6H7O2S3+·BF4−, 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 ethylenedioxy group fused at the 4,5-positions; the ethylenedioxy 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 interactions [3.022 (4–3.095 (4 Å] and an S...O [3.247 (4 Å] interaction are present.

1-(4-Methylphenylsulfonyl-5,6-dinitro-1H-indazole

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Bassou Oulemda

2014-01-01

Full Text Available In the title compound, C14H10N4O6S, the indazole ring system is almost perpendicular to the tosyl ring, as indicated by the dihedral angle of 89.40 (9° between their planes. The dihedral angles between the indazole system and the nitro groups are 57.0 (3 and 31.9 (3°. In the crystal, molecules are linked by C—H...O interactions, forming chains running along [100].

Photochemically activated antiviral halogenated 1,8-naphthalimides: synthesis of N,N'-bis-{2-[(5-bromo-2-[1-14C]hexyl-1H-benz[de]isoquinolin-1,3(2H)-dion-6-yl)amino]ethyl}hexanediamide

International Nuclear Information System (INIS)

Hayes, B.A.; Gupta, Surendra; Shaochieh Chang; Utecht, R.E.; Lewis, D.E.

1996-01-01

The synthesis of N,N'-bis-{2-[(5-bromo-2-[1- 14 C]hexyl-1H-benz[de]isoquinolin-1, 3(2H)-dion-6-yl)amino]ethyl}hexanediamide from 1-[1- 14 C]-hexylamine and 4-chloro-1,8-naphthalic anhydride is described. The anhydride is first converted to the 4-chloro-n-[1- 14 C]hexyl-1,8-naphthalimide by condensation with 1-[1- 14 C]-hexylamine, and the chlorine is then displaced with ethylenediamine to give the 4-(2-aminoethylamino-N-[1- 14 C]hexyl-1,8-naphthalimide. Coupling of this monomeric naphthalimide with adipoyl chloride affords the dimeric naphthalimide which is brominated regiospecifically with elemental bromine in carbon tetrachloride to afford the title compound. (author)

Synthesis of 7-[α-(2-amino-[2-14C]thiazol-4-yl)-α-(Z)-methoxyimin oacetamido]-3-(1-methylpyrrolidinio)methyl-3-cephem-4-carboxylate hydrochloride ([14C]cefepime hydrochloride)

International Nuclear Information System (INIS)

Standridge, R.T.; Swigor, J.E.

1993-01-01

The title compound ([ 14 C]cefepime hydrochloride) was prepared as follows:- [ 14 C]Thiourea was condensed with ethyl 4-bromo-3-oxo-2-methoxyimino-acetate providing ethyl 2-(2-amino-4-[2- 14 C] thiazolyl)-2-methoxyi-minoacetate as the pure Z-isomer. Saponification gave the amino acid this was reacted with 1-hydroxybenzotriazole to give the activated ester. Condensation in situ with 7-amino-3-(1-methylpyrrolidinio) methyl-3-cephem-4-carboxylate yielded the product as the pure sulfate salt. Treatment of the sulfate salt with base provided the zwitterion isolated as the stable N-methyl-2-pyrrolidinone adduct. An aqueous solution of the adduct was converted to the crystalline title compound, [ 14 C]Cefepime hydrochloride hydrate, with hydrochloric acid/acetone. Radiochemical purity was 99.0% and specific activity, 34.2 μCi/mg. Overall yield from [ 14 C]thiourea was 18%. (Author)

Sensitive method for continuous air monitoring for /sup 14/C and /sup 3/H. Empfindliches verfahren zur koninuierlichen C-14 und H-3 luftueberwachung

Energy Technology Data Exchange (ETDEWEB)

Rudolph, J.; Weiss, W.

1976-07-01

In the monitoring of air for /sup 14/C and /sup 3/H the necessary sensitivity cannot be achieved by direct measurement, but only through continuous sampling and scintillation spectroscopy. The two radionuclides are separated from each other at the time of sampling. In addition, by a catalytic reaction over CuO at 600/sup 0/C, a differentiation is achieved between tritiated atmospheric water vapor (HTO), /sup 14/CO/sub 2/ and other isotopically labeled substances contained in the air. Tritium is obtained in the form of water and /sup 14/C as Na/sub 2//sup 14/CO/sub 3/. Radioactivity is measured in a scintillation spectrometer. For tritium this method has a detection limit of 0.8 pCi/m/sup 3/ or air, and for C/sup 14/ 0.6 pCi/m/sup 3/ of air. These values correspond to 15 to 30% of the mean background concentration for HTO and /sup 14/CO/sub 2/ observed up to the present.

Synthesis and crystal structure of new uranyl selenite(IV)-selenate(VI) [C5H14N][(UO2)3(SeO4)4(HSeO3)(H2O)](H2SeO3)(HSeO4)

International Nuclear Information System (INIS)

Krivovichev, S.V.; Tananaev, I.G.; Myasoedov, B.F.; Kalenberg, V.

2006-01-01

Crystals of new uranyl selenite(IV)-selenate(VI) [C 5 H 14 N][(UO 2 ) 3 (SeO 4 ) 4 (HSeO 3 )(H 2 O)](H 2 SeO 3 )(HSeO 4 ) are obtained by the method of evaporation from aqueous solutions. Compound has triclinic lattice, space group P1-bar, a=11.7068(9), b=14.8165(12), c=16.9766(15), α=73.899(6), β=76.221(7), γ=89.361(6) Deg, V=2743.0(4) A 3 , Z=2. Laminated complexes (UO 2 ) 3 (SeO 4 ) 4 (HSeO 3 )(H 2 O)] 3- are the basis of the structure. [HSe(VI)O 4 ] - , [H 2 Se(IV)O 3 ] complexes and protonated methylbutylamine cations are disposed between layers [ru

meso-4,4′-Dimethoxy-2,2′-{[(3aR,7aS-2,3,3a,4,5,6,7,7a-octahydro-1H-benzimidazole-1,3-diyl]bis(methylene}diphenol

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Augusto Rivera

2013-07-01

Full Text Available The title compound, C23H30N2O4, a di-Mannich base derived from 4-methoxyphenol and cis-1,2-diaminecyclohexane, has a perhydrobenzimidazolidine nucleus, in which the cyclohexane ring adopts a chair conformation and the heterocyclic ring has a half-chair conformation with a C—N—C—C torsion angles of −48.14 (15 and −14.57 (16°. The mean plane of the heterocycle makes dihedral angles of 86.29 (6 and 78.92 (6° with the pendant benzene rings. The molecular structure of the title compound shows the presence of two interactions between the N atoms of the imidazolidine ring and the hydroxyl groups through intramolecular O—H...N hydrogen bonds with graph-set motif S(6. The unobserved lone pairs of the N atoms are presumed to be disposed in a syn conformation, being only the second example of an exception to the typical `rabbit-ears' effect in 1,2-diamines.

Crystal structure and thermochemical properties of n-decylammonium ethyl sulfate (C10H21NH3SO4C2H5)(s)

International Nuclear Information System (INIS)

Zhang, Li-Jun; Di, You-Ying; Dou, Jian-Min

2013-01-01

Graphical abstract: Crystal structure of n-decylammonium ethyl sulfate was determined by X-ray crystallography. Lattice potential energy and molar volume of the solid compound and its anion were respectively obtained. Molar enthalpies of dissolution of the compound at different concentrations were measured by an isoperibol solution–reaction calorimeter. According to the Pitzer’s electrolyte solution theory, molar enthalpy of dissolution of the compound at infinite dilution and Pitzer parameters were obtained. The values of apparent relative molar enthalpies of the title compound and relative partial molar enthalpies of the solute and the solvent at different concentrations were derived. Finally, enthalpies of hydration of the compound and its anion were calculated. Highlights: ► Crystal structure of n-decylammonium ethyl sulfate was determined. ► Lattice potential energy was calculated. ► Molar enthalpy of dissolution at infinite dilution was determined. ► Enthalpies of hydration of the compound and its anion were derived. - Abstract: Crystal structure of n-decylammonium ethyl sulfate was determined by X-ray crystallography. Lattice potential energy and molar volume of the solid compound and its anion were respectively obtained. Ionic radius of the anion was calculated from the corresponding effective volume of the anion. Molar enthalpies of dissolution of the compound at different concentrations m /(mol · kg –1 ) were measured by an isoperibol solution–reaction calorimeter at T = 298.15 K. According to the Pitzer’s electrolyte solution theory, molar enthalpy of dissolution of the compound at infinite dilution (Δ sol H m ∞ ) was determined to be (21.284 ± 0.042) kJ·mol –1 , and enthalpy of hydration of the anion SO 4 C 2 H 5 − was calculated to be ΔH – = −340.68 kJ·mol –1 . The values of apparent relative molar enthalpies ( Φ L) of the title compound and relative partial molar enthalpies (L 2 ¯ and L 1 ¯ ) of the solute and

4-{3-[Hydroxy(phenylmethyl]-5-thioxo-4,5-dihydro-1H-1,2,4-triazol-4-yl}benzenesulfonamide

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Mehmet Akkurt

2010-04-01

Full Text Available In the title compound, C15H14N4O3S2, the hydroxy group is disordered over two positions with occupancies of 0.619 (5 and 0.381 (5. The benzene ring attached to the heterocycle makes a dihedral angle of 86.92 (9° with respect to the best plane through the five-membered ring. The crystal packing is stabilized by intermolecular O—H...O, N—H...S, N—H...N, C—H...O and C—H...N hydrogen bonds, and N—H...π and C—H...π interactions.

Ethyl 4-chloro-2′-fluoro-3-hydroxy-5-methylbiphenyl-2-carboxylate

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Muhammad Adeel

2011-09-01

Full Text Available In the title compound, C16H14ClFO3, the dihedral angle between the mean planes of the two benzene rings is 71.50 (5°. Due to an intramolecular O—H...O hydrogen bond between the hydroxy group and the carbonyl O atom of the ethyl ester group, the ethyl ester group lies within the ring plane. The crystal structure is consolidated by intermolecular C—H...O and C—H...F interactions.

Synthesis of 1-amino-2-[3-(3-[2,6-14C]piperidinomethylphenoxy) propylamino]-1-cyclobutene-3,4-dione hydrochloride

International Nuclear Information System (INIS)

Swigor, J.E.; Algieri, A.A.; Standridge, R.T.; Pittman, K.A.

1985-01-01

The synthesis of the title compound is described. The condensation of 3-aminopropanol with phthalic anhydride and subsequent treatment with phosphorous tribromide produced N-[3-bromopropyl] phthalimide. Acylation with 3-hydroxybenzaldehyde, reduction with hydrogen over Raney nickel and subsequent treatment with thionyl chloride gave N-[3-(3-chloromethylphenoxy) propyl] phthalimide. Treatment with [2,6 - 14 C] piperidine introduced the radiolabel. Deprotection of the amino group with hydrazine and treatment with 3-methoxy-4-amino-3-cyclobutene-1,2-dione produced 1-amino-2-[3-(3-[2,6- 14 C]piperidinomethylphenoxy) propylamino]-1-cyclobutene-3, 4-dione. Treatment with hydrochloric acid yielded the title compound in an overall chemical yield of 22%. (author)

Synthesis of [3,5-14C]trachelanthamidine and [5-3H]isoretronecanol and their incorporation into the retronecine moiety of riddelliine in Senecio riddellii

International Nuclear Information System (INIS)

Leete, E.; Rana, J.

1986-01-01

(+/-)-[3,5- 14 C]Trachelanthamidine and (+/-)-[5- 3 H]isoretronecanol, which are diastereomers, were prepared from potassium [ 14 C]cyanide and [5- 3 H]proline, respectively. These compounds and [1,4- 14 C]putrescine were administered to Senecio riddellii plants resulting in the formation of labeled riddelliine, in which almost all the radioactivity was located in its retronecine moiety. The activity of the beta-alanine obtained by degradation of the retronecine was consistent with specific labeling of this pyrrolizidine base at the expected positions. The extremely high absolute incorporation (15.1, 22.1%) of trachelanthamidine into riddelliine strongly favors this 1-hydroxymethylpyrrolizidine as the one on the main biosynthetic pathway to retronecine. The lower incorporation (0.75%) of isoretronecanol may represent a minor or aberrant pathway to retronecine

Primary assimilation process of triply (/sup 15/N, /sup 14/C and /sup 3/H) labeled arginine in the roots of arginine-fed barley

Energy Technology Data Exchange (ETDEWEB)

Mori, Satoshi [Tokyo Univ. (Japan). Faculty of Agriculture

1981-03-01

To clarify the mechanism of arginine utilization in barley roots, triply labeled (ureido-/sup 15/N, ureido-/sup 14/C and 5-/sup 3/H) arginine was applied to plants precultured with arginine (Arg-plants). (5-/sup 3/H) Arginine was incorporated mainly into ornithine, suggesting that arginase contributes in the first step of arginine metabolism. The arginase activity in the tissues was greatly enhanced by continuous supply of arginine, whereas urease activity was not by the same treatment. The amount of /sup 14/CO/sub 2/ evolved from (ureido-/sup 14/C) arginine in the Arg-plants was several times higher than that in plants treated with NO/sub 3//sup -/(NO/sub 3/-plants), and most /sup 14/C-urea exogenously supplied to detached roots of Arg-plants was immediately decomposed to /sup 14/CO/sub 2/. The urea released from arginine by arginase was cleaved to /sup 15/NH/sub 4//sup +/ + /sup 14/CO/sub 2/ by urease. Most of the /sup 14/CO/sub 2/ was then lost from the root system. On the other hand, the released /sup 15/NH/sub 4//sup +/ was reassimilated into amino acids probably through the pathway of ammonia assimilation. Released (5-/sup 3/H) ornithine was metabolized dominantly to proline.

(S-2-(2-Pyrrolidinio-1H-benzimidazol-3-ium dichloride monohydrate

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Dai Jing

2009-06-01

Full Text Available In the title compound, C11H15N32+·2Cl−·H2O, one N atom of the imidazole ring and the N atom of the pyrrolidine ring are protonated. The crystal structure is stabilized by aromatic π–π interactions between the benzene rings of neighbouring benzimidazole systems [centroid–centroid duistance = 3.712 (2 Å]. The crystal structure is further stabilized by intermolecular N—H...Cl, O—H...Cl and N—H...O hydrogen bonds.

1-(2-Ethoxy-2-methyl-2H-chromen-3-ylethanone

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Afsaneh Zonouzi

2009-04-01

Full Text Available The Csp3 atom of the chromenyl fused-ring system in the title compound, C14H16O3, deviates by 0.407 (2 Å from the plane of the other atoms (r.m.s. deviation = 0.041 Å. The ethoxy substituent occupies a pseudo-axial position.

(S-2-(4-Chlorobenzoyl-1,2,3,4-tetrahydrobenzo[e]pyrazino[1,2-a][1,4]diazepine-6,12(11H,12aH-dione—Synthesis and Crystallographic Studies

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Adam Mieczkowski

2017-10-01

Full Text Available (S-2-(4-Chlorobenzoyl-1,2,3,4-tetrahydrobenzo[e]pyrazino[1,2-a][1,4]diazepine-6,12(11H,12aH-dione was obtained in a three-step, one-pot synthesis, starting from optically pure (S-2-piperazine carboxylic acid dihydrochloride. Selective acylation of the β-nitrogen atom followed by condensation with isatoic anhydride and cyclization with HATU/DIPEA to a seven-member benzodiazepine ring, led to the tricyclic benzodiazepine derivative. Crystallographic studies and initial biological screening were performed for the title compound.

A Facile Synthesis of Pyrido[2′,3′:3,4]pyrazolo[1,5-a]pyrimidine and Pyrido[2′,3′:3,4]pyrazolo[5,1-c][1,2,4]triazine Bearing a Thiophene Moiety

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Tilal Elsaman

2013-01-01

Full Text Available Pyridinone derivative 8 was synthesized and transformed into the respective chloropyridine 9, which was allowed to react with hydrazine hydrate to afford pyrazolo[3,4-b]pyridin-3-amine derivative 11. Compound 11 was used as a key intermediate for a facile synthesis of the title compounds 14, 15, 17, 21a,b, and 24a–c where the reaction of 11 with some 1,3-dielecrophiles resulted in the formation of pyrido[2′,3′:3,4]pyrazolo[1,5-a]pyrimidines 14, 15, and 17, whereas diazotization of compound 11 gave the respective diazonium salt 18 which was coupled with some active methylene-containing compounds to give the corresponding hydrazones 19a,b and 22a–c. Cyclization of the latter hydrazones yielded the pyrido[2′,3′:3,4]pyrazolo[5,1-c][1,2,4]triazines 21a,b and 24a–c, respectively.

2-(5-Fluoro-3-methylsulfanyl-1-benzofuran-2-ylacetic acid

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Hong Dae Choi

2009-08-01

Full Text Available The title compound, C11H9FO3S, was prepared by alkaline hydrolysis of ethyl 2-(5-fluoro-3-methylsulfanyl-1-benzofuran-2-ylacetate. In the crystal structure, the carboxyl groups are involved in intermolecular O—H...O hydrogen bonds, which link the molecules into centrosymmetric dimers. These dimers are further packed into stacks along the b axis by intermolecular C—H...O and C—H...F interactions.

(3aS,7aS-5-[(S-3,3,3-Trifluoro-2-methoxy-2-phenylpropanoyl]-2,3,4,5,6,7-hexahydro-1H-pyrrolo[3,4-c]pyridin-3(2H-one monohydrate

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Huichun Zhu

2010-01-01

Full Text Available rac-Benzyl 3-oxohexahydro-1H-pyrrolo[3,4-c]pyridine-5(6H-carboxylate was separated by chiral chromatography, and one of the enantiomers ([α]22D = +10° was hydrogenated in the presence of Pd/C in methanol, producing octahydro-3H-pyrrolo[3,4-c]pyridin-3-one. The latter was reacted with (2R-3,3,3-trifluoro-2-methoxy-2-phenylpropanoyl chloride [(R-(−-Mosher acid chloride], giving rise to the title compound, C17H19F3N2O3·H2O. The present structure established the absolute configuration of the pyrrolopiperidine fragment based on the known configuration of the (R-Mosher acid chloride. The piperidine ring has a somewhat distorted chair conformation and is cis-fused with the five-membered envelope-shaped ring; the plane of the exocyclic amide bond is approximately orthogonal to the plane of the phenyl ring, making a dihedral angle of 82.31 (3°. The water molecule acts as an acceptor to the proton of the amino group in an N—H...O interaction, and as a double proton donor in O—H...O hydrogen bonds, generating infinite bands along the a axis.

Vibrational spectroscopic (FT-IR, FT-Raman) and quantum mechanical study of 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno[3,2-f] [1,2,4]triazolo[4,3-a][1,4] diazepine

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Kuruvilla, Tintu K.; Prasana, Johanan Christian; Muthu, S.; George, Jacob

2018-04-01

The spectroscopic properties of 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno [3,2-f] [1,2,4] triazolo [4,3-a] [1,4] diazepine were investigated in the present study using FT-IR and FT-Raman techniques. The results obtained were compared with quantum mechanical methods, as it serves as an important tool in interpreting and predicting vibrational spectra. The optimized molecular geometry, the vibrational wavenumbers, the infrared intensities and Raman scattering were calculated using density functional theory B3LYP method with 6-311++g (d,p) basis set. All the experimental results were in line with the theoretical data. The molecular electrostatic potential (MEP) and HOMO LUMO energies of the title compound were accounted. The results indicated that the title compound has a lower softness value (0.27) and high electrophilicity index (4.98) hence describing its biological activity. Further, natural bond orbital was also analyzed as part of the work. Fukui functions were calculated in order to explain the chemical selectivity or the reactivity site in 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno [3,2-f] [1,2,4] triazolo [4,3-a] [1,4] diazepine. The thermodynamic properties of the title compound were closely examined at different temperatures. It revealed the correlations between heat capacity (C), entropy (S) and enthalpy changes (H) with temperatures. The paper further explains that the title compound can act as good antidepressant through molecular docking studies.

(2E)-3-[4-(Benz-yloxy)phen-yl]-1-(2,6-dichloro-3-fluoro-phen-yl)prop-2-en-1-one.

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Praveen, Aletti S; Yathirajan, Hemmige S; Gerber, Thomas; van Brecht, Benjamin; Betz, Richard

2012-12-01

In the title compound, C22H15Cl2FO2, a chalcone derivative featuring a threefold-halogenated aromatic substituent, the conformation about the C=C bond is E. In the crystal C-H⋯F and C-H⋯Cl contacts connect the mol-ecules into undulating sheets parallel to (101). In addition, C-H⋯π inter-actions are also present.

5-[(E-(2-Hydroxybenzylideneamino]-1H-1,3-benzimidazole-2(3H-thione

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Hoong-Kun Fun

2011-01-01

Full Text Available There are two molecules in the asymmetric unit of the title compound, C14H11N3OS. In each, the benzimidazole ring system is essentially planar, with maximum deviations of 0.010 (2 and 0.006 (2 Å, and makes dihedral angles of 8.70 (9 and 13.75 (8°, respectively, with the hydroxy-substituted benzene rings. Each molecule adopts an E configuration about the central C=N double bond. In the crystal, the two independent molecules are connected via intermolecular N—H...S hydrogen bonds, forming dimers. Furthermore, the dimers are connected by N—H...O hydrogen bonds into molecular ribbons along the c axis. There is an intramolecular O—H...N hydrogen bond in each molecule, which generates an S(6 ring motif.

Solvent-Dependent Delamination, Restacking, and Ferroelectric Behavior in a New Charge-Separated Layered Compound: [NH4 ][Ag3 (C9 H5 NO4 S)2 (C13 H14 N2 )2 ]⋅8 H2 O.

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Sushrutha, Sringeri Ramesh; Mohana, Shivanna; Pal, Somnath; Natarajan, Srinivasan

2017-01-03

A new anionic coordination polymer, [NH 4 ][Ag 3 (C 9 H 5 NO 4 S) 2 (C 13 H 14 N 2 ) 2 ]⋅8 H 2 O, with a two-dimensional structure, has been synthesized by a reaction between silver nitrate, 8-hydroxyquinoline-5-sulfonic acid (HQS), and 4,4'-trimethylene dipyridine (TMDP). The compound stabilizes in a noncentrosymmetric space group, and the lattice water molecules and the charge-compensating [NH 4 ] + group occupy the inter-lamellar spaces. The lattice water molecules can be fully removed and reinserted, which is accompanied by a crystalline-amorphous-crystalline transformation. This transformation resembles the collapse/delamination and restacking of the layers. To the best of our knowledge, this is the first observation of delamination and restacking in an inorganic coordination polymer that contains silver. The presence of a natural dipole (the anionic framework and cationic ammonium ions) along with the noncentrosymmetric space group gives rise to the room-temperature ferroelectric behavior of the compound. The ferroelectric behavior is also water-dependent and exhibits a ferroelectric-paraelectric transformation. The temperature-dependent dielectric measurements indicate that the ferroelectric/ paraelectric transformation occurs at 320 K. This transformation has also been investigated by using in-situ IR spectroscopy and PXRD studies. The second-harmonic generation (SHG) study indicated values that are comparable to some of the known SHG solids, such as potassium dihydrogen phosphate (KDP) and urea. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

2-Oxo-2H-chromen-3-yl benzoate

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Konan René Kambo

2017-05-01

Full Text Available In the title compound, C16H10O4, the dihedral angle between the coumarin ring system (r.m.s. deviation = 0.015 Å and the benzoate group is 83.58 (9°, which compares to a value of 81.8° obtained from a DFT calculation at the B3LYP/6–311 G(d,p level. In the crystal, C—O...π and C—H...π interactions and aromatic π–π [Cg...Cg = 3.7214 (14 and 3.7059 (14 Å] stacking generate a three-dimensional network.

4-((E-{2-[N-(1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylcarboximidoyl]benzylidene}amino-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one

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Richard Betz

2011-10-01

Full Text Available The title compound, C30H28N6O2, is a symmetric diimine derived from ortho-dibenzaldehyde. Both C=N bonds are (E-configured. The terminal N-bonded phenyl groups adopt staggered conformations relative to their respective parent heterocycles, the relevant least-squares planes intersect at angles of 32.35 (11 and 38.59 (10°. In the crystal, C—H...O contacts connect the molecules into chains along the b axis and give rise to a C11(14C11(14 and a R22(12 pattern on different levels of graph-set analysis. The shortest intercentroid distance between two centroids was found at 4.2074 (11 Å between the two five-membered heterocycles.

(5S,6R-6-Bromo-6-methyl-5-phenyl-3,4,5,6-tetrahydro-2H-cyclopenta[b]pyran-7-one

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Winai Ieawsuwan

2011-10-01

Full Text Available The title compound, C15H15BrO2, was synthesized by a Brønsted acid-catalysed domino electrocyclization-halogenation reaction. The five-membered ring is essentially planar (r.m.s. deviation 0.006 Å and forms a dihedral angle of 72.7 (3° with the attached phenyl ring. The six-membered heterocycle adopts a half-chair conformation. The crystal packing is stabilized by a C—H...O contact.

Synthesis of 14C- and 3H-labelled 4-(4-nitrophenyl)aminophenylisothiocyanate (Go 9333/CGP 4540; amoscanate)

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Anjaneyulu, B.; Maller, R.K.; Nagarajan, K.

1985-01-01

Amoscanate, a broad spectrum anthelmintic, labelled with carbon-14 on the isothiocyanate carbon atom was prepared in an overall yield of 13% at a specific activity of 4.13 μCi/mg from potassium [ 14 C]thiocyanate. The 4-nitro[U- 14 C]phenyl ring labelled compound was synthesized in 20.4% overall yield from [U- 14 C]aniline at a specific activity of 12.2 μCi/mg. The corresponding tritiated compound was prepared from 4-amino[2- 3 H]acetanilide at 112 μCi/mg. Labelling with tritium in the aromatic ring bearing the isothiocyanate group was achieved by catalysed halogen-tritium replacement. However, for pharmacokinetic and metabolism studies in experimental animals, the 14 C- and 3 H-labels associated with the phenylisothiocyanate moiety subsequently proved disadvantageous because of the instability of the labels in vivo. (author)

6-Methoxy-1-(4-methoxyphenyl-1,2,3,4-tetrahydro-9H-β-carbolin-2-ium acetate

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Mohd Mustaqim Rosli

2012-05-01

Full Text Available In the title compound, C19H21N2O2+·C2H3O2−, the 1H-indole ring system is essentially planar [maximum deviation = 0.0257 (14 Å] and forms a dihedral angle of 87.92 (7 Å with the benzene ring attached to the tetrahydropyridinium fragment. The tetrahydropyridinium ring adopts a half-chair conformation. In the crystal, cations and anions are linked by interionic N—H...O, C—H...O and C—H...N hydrogen bonds into chains along the a axis.

8-Chloro-4-oxo-4H-chromene-3-carbaldehyde

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Yoshinobu Ishikawa

2014-07-01

Full Text Available In the title compound, C10H5ClO3, a chlorinated 3-formylchromone derivative, all atoms are essentially coplanar (r.m.s. deviation = 0.032 Å for the non-H atoms, with the largest deviation from the least-squares plane [0.0598 (14 Å] being for a pyran-ring C atom. In the crystal, molecules are linked through stacking interactions along the b axis [shortest centroid–centroid distance between the pyran and benzene rings = 3.566 (2 Å].

(2E)-1-(2,6-Dichloro-3-fluoro-phen-yl)-3-phenyl-prop-2-en-1-one.

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Praveen, Aletti S; Yathirajan, Hemmige S; Narayana, Badiadka; Gerber, Thomas; Hosten, Eric; Betz, Richard

2012-04-01

In the title compound, C(15)H(9)Cl(2)FO, the F atom shows positional disorder over two positions, with site-occupancy factors of 0.747 (4) and 0.253 (4). The dihedral angle between the rings is 86.37 (10)°. In the crystal, C-H⋯O contacts connect the mol-ecules into chains along the c axis. The shortest inter-centroid distance between two aromatic systems is 3.6686 (12) Å and is apparent between the halogenated rings.

Synthesis of (3,5-/sup 14/C)trachelanthamidine and (5-/sup 3/H)isoretronecanol and their incorporation into the retronecine moiety of riddelliine in Senecio riddellii

Energy Technology Data Exchange (ETDEWEB)

Leete, E.; Rana, J.

1986-09-01

(+/-)-(3,5-/sup 14/C)Trachelanthamidine and (+/-)-(5-/sup 3/H)isoretronecanol, which are diastereomers, were prepared from potassium (/sup 14/C)cyanide and (5-/sup 3/H)proline, respectively. These compounds and (1,4-/sup 14/C)putrescine were administered to Senecio riddellii plants resulting in the formation of labeled riddelliine, in which almost all the radioactivity was located in its retronecine moiety. The activity of the beta-alanine obtained by degradation of the retronecine was consistent with specific labeling of this pyrrolizidine base at the expected positions. The extremely high absolute incorporation (15.1, 22.1%) of trachelanthamidine into riddelliine strongly favors this 1-hydroxymethylpyrrolizidine as the one on the main biosynthetic pathway to retronecine. The lower incorporation (0.75%) of isoretronecanol may represent a minor or aberrant pathway to retronecine.

Low-temperature heat capacity and standard molar enthalpy of formation of 9-fluorenemethanol (C14H12O)

International Nuclear Information System (INIS)

Di, You-Ying; Tan, Zhi-Cheng.; Sun, Xiao-Hong; Wang, Mei-Han; Xu, Fen; Liu, Yuan-Fa; Sun, Li-Xian; Zhang, Hong-Tao

2004-01-01

Low-temperature heat capacities of the 9-fluorenemethanol (C 14 H 12 O) have been precisely measured with a small sample automatic adiabatic calorimeter over the temperature range between T=78 K and T=390 K. The solid-liquid phase transition of the compound has been observed to be T fus =(376.567±0.012) K from the heat-capacity measurements. The molar enthalpy and entropy of the melting of the substance were determined to be Δ fus H m =(26.273±0.013) kJ · mol -1 and Δ fus S m =(69.770±0.035) J · K -1 · mol -1 . The experimental values of molar heat capacities in solid and liquid regions have been fitted to two polynomial equations by the least squares method. The constant-volume energy and standard molar enthalpy of combustion of the compound have been determined, Δ c U(C 14 H 12 O, s)=-(7125.56 ± 4.62) kJ · mol -1 and Δ c H m compfn (C 14 H 12 O, s)=-(7131.76 ± 4.62) kJ · mol -1 , by means of a homemade precision oxygen-bomb combustion calorimeter at T=(298.15±0.001) K. The standard molar enthalpy of formation of the compound has been derived, Δ f H m compfn (C 14 H 12 O,s)=-(92.36 ± 0.97) kJ · mol -1 , from the standard molar enthalpy of combustion of the compound in combination with other auxiliary thermodynamic quantities through a Hess thermochemical cycle

NCI calculations for understanding a physical phase transition in (C6H14N2)[Mn(H2O)6](SeO4)2

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Naïli, Houcine; François, Michel; Norquist, Alexander J.; Rekik, Walid

2017-12-01

An organically templated manganese selenate, (C6H14N2)[Mn(H2O)6](SeO4)2, has been synthesized by slow evaporation and crystallographically characterized. The title compound crystallizes at room temperature in the monoclinic centrosymmetric space group P21/n, with the following unit cell parameters: a = 7.2373(4) Å; b = 12.5600(7) Å; c = 10.1945(7) Å; β = 91.155(4)°, V = 926.50(10) Å3and Z = 2. Its crystal structure is built of manganese(II) cations coordinated by six water molecules in octahedral geometry, disordered dabcodiium cations and selenate anions, resulting in an extensive hydrogen-bonding network. Differential scanning calorimetry (DSC) measurement indicated that the precursor undergoes a reversible phase transition at about 216 and 218 K during the cooling and heating processes respectively. Below this temperature the title compound is noncentrosymmetric with space group P21 and lattice parameters a = 7.2033(8) Å; b = 12.4981(13) Å; c = 10.0888(11) Å; β = 91.281(2)°, V = 908.04(17) Å3 and Z = 2. The disorder-order transformation of the C atoms of (C6H14N2)2+ cation may drive the structural phase transition. The low temperature phase obtained by breaking symmetry presents a fully ordered structure. The noncovalent interaction (NCI) method was used not only to locate, quantify, and visualize intermolecular interactions in the high and low temperature phases but also to confirm the phase transition detected by DSC measurement. The thermal decomposition of this new compound proceeds through four stages giving rise to the manganese oxide as final product at 850 °C.

4-{(E-[2-(4-Iodobutoxybenzylidene]amino}-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one

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Hoong-Kun Fun

2010-07-01

Full Text Available The title Schiff base compound, C22H24IN3O2, adopts an E configuration about the central C=N bond. The pyrazolone ring makes a dihedral angle of 49.68 (10° with its attached phenyl ring. The phenolate plane makes dihedral angles of 16.78 (9 and 50.54 (9°, respectively, with the pyrazolone ring and the terminal phenyl ring. An intramolecular C—H...O hydrogen bond generates an S(6 ring motif. In the crystal structure, an intermolecular C—H...O hydrogen bond is also observed.

(Carbonyl-1κC)bis­[2,3(η5)-cyclo­penta­dien­yl][μ3-(S-methyl trithio­carbonato)methylidyne-1:2:3κ4 C,S′′:C:C](triphenyl­phosphine-1κP)(μ3-sulfido-1:2:3κ3 S)dicobalt(II)iron(II) trifluoro­methane­sulfonate

Science.gov (United States)

Manning, Anthony R.; McAdam, C. John; Palmer, Anthony J.; Simpson, Jim

2008-01-01

The asymmetric unit of the title compound, [FeCo2(C5H5)2(C3H3S3)S(C18H15P)(CO)]CF3SO3, consists of a triangular irondicobalt cluster cation and a trifluoro­methane­sulfonate anion. In the cation, the FeCo2 triangle is symmetrically capped on one face by an S atom and on the other by a C atom linked to a methyl trithio­carbonate residue that bridges the Fe—C bond. Each Co atom carries a cyclo­penta­dienyl ligand while the Fe atom coordinates to one carbonyl and one triphenyl­phosphine ligand. In the crystal structure, the cation is linked to the anion by a number of weak non-classical C—H⋯O and C—H⋯F hydrogen bonds and weak S⋯O (3.317 Å) and S⋯F (3.198 Å) inter­actions. The structure is further stabilized by additional inter­molecular C—H⋯O, C—H⋯F and O⋯O (2.942 Å) contacts, together with an unusual S⋯π(Cp) inter­action (S⋯centroid distance = 3.385 Å), generating an extended network. PMID:21202187

Synthesis of [14α, 15α-3H]-norgestrel

International Nuclear Information System (INIS)

Wagner, H.

1988-01-01

The preparation of the well-known gestogen norgestrel in a tritium labelled form is described. Starting material was 18-methyl-3-methoxy-estra-1,3,5(10),8,14-pentaen-17β-o1 acetate. In a four step synthesis 17α-ethinyl-17β-hydroxy-18-methyl-[14α,15α- 3 H]-estr-4-en-3-one was obtained with a specific activity of 52 Ci/mmol and a radiochemical purity > 99%. (author)

4-[(3-Phenyl-4,5-dihydroisoxazol-5-ylmethyl]-2H-benzo[b][1,4]thiazin-3(4H-one

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Nada Kheira Sebbar

2016-06-01

Full Text Available In the title compound, C18H16N2O2S, the 5-dihydroisoxazol-5-yl ring and its phenyl substituent are nearly coplanar, with the largest deviation from the mean plane being 0.0184 (16 Å. The thiomorpholin-3-one ring adopts a screw-boat conformation and the attached benzene ring makes a dihedral angle of 42.26 (7° with the mean plane through the 3-phenyl-4,5-dihydroisoxazol-5-yl ring system. In the crystal, molecules are linked by pairs of C—H...N hydrogen bonds, forming inversion dimers. These dimers are linked via C—H...O hydrogen bonds, generating a three-dimensional network.

2-(4-Fluoroanilino-3-(2-hydroxyethylquinazolin-4(3H-one

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2009-03-01

Full Text Available The molecular and crystal structures of the title compound, C16H14FN3O2, are stabilized by intramolecular N—H...O and intermolecular O—H...O hydrogen bonds. The existence of non-classical intramolecular C—H...N hydrogen bonds provides a dihedral angle between the fluoro-substituted benzene and pyrimidinone rings of 7.9 (1°.

Crystal structure of (E-2-benzylidene-4-[(3-phenyl-4,5-dihydroisoxazol-5-ylmethyl]-2H-benzo[b][1,4]thiazin-3(4H-one

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Nada Kheira Sebbar

2015-06-01

Full Text Available In the title compound, C25H20N2O2S, the dihydroisoxazole ring exhibits an envelope conformation with the methine atom being the flap, while the 1,4-thiazine ring displays a screw-boat conformation. The six-membered ring fused to the 1,4-thiazine ring makes dihedral angles of 63.04 (2 and 54.7 (2° with the mean planes through the five-membered heterocycle and the attached phenyl ring, respectively. The phenyl group connected to the 1,4-thiazine ring is disordered over two sites [major component = 0.57 (2]. The most prominent interactions in the crystal structure are C—H...O hydrogen bonds that link molecules, forming inversion dimers, and C—H...N hydrogen bonds that link the dimers into columns parallel to the b axis.

The Co-III-C bond in (1-thia-4,7-diazacyclodecyl-kappa N-3(4),N-7,C-10)(1,4,7-triazacyclononane-kappa N-3(1),N-4,N-7)-cobalt(III) dithionate hydrate

DEFF Research Database (Denmark)

Harris, Pernille; Kofod, P.; Song, Y.S.

2003-01-01

In the title compound, [Co(C6H15N3)(C7H15N2S)]S2O6.H2O, the Co-C bond distance is 1.9930 (13) Angstrom, which is shorter than for related compounds with the linear 1,6-diamino-3-thiahexan-4-ide anion in place of the macrocyclic 1-thia-4,7-diazacyclodecan-8-ide anion. The coordinated carbanion pro...... produces an elongation of 0.102 (7) Angstrom of the Co-N bond to the 1,4,7-triazacyclononane N atom in the trans position. This relatively small trans influence is presumably a result of the triamine ligand forming strong bonds to the Co-III atom....

Crystal structure of [(2R,3R,4S)-3,4-bis(acet-yloxy)-5-iodo-3,4-di-hydro-2H-pyran-2-yl]methyl acetate.

Science.gov (United States)

Zukerman-Schpector, Julio; Caracelli, Ignez; Stefani, Hélio A; Shamim, Anwar; Tiekink, Edward R T

2015-01-01

In the title compound, C12H15IO7, the 3,4-di-hydro-2H-pyran ring is in a distorted half-boat conformation with the atom bearing the acet-yloxy group adjacent to the C atom bearing the methyl-acetate group lying 0.633 (6) Å above the plane of the remaining ring atoms (r.m.s. deviation = 0.0907 Å). In the crystal, mol-ecules are linked into a supra-molecular chain along the a axis through two C-H⋯O inter-actions to the same acceptor carbonyl O atom; these chains pack with no specific inter-molecular inter-actions between them.

Synthesis of 14C- and 3H-labeled fluoxetine, a selective serotonin uptake inhibitor

International Nuclear Information System (INIS)

Robertson, D.W.; Krushinski, J.H.; Wong, D.T.; Kau, D.

1987-01-01

Fluoxetine (N-methyl-γ-(4-(trifluoromethyl)phenoxy) benzenepropanamine) is a potent, highly selective serotonin uptake inhibitor that is useful in treating a variety of major psychiatric derangements. We have synthesized this compound in 14 C- and 3 H-labeled forms. The tritium label was introduced in the final step by catalytic dehalogenation of the brominated fluoxetine precursor. Reaction conditions could be controlled such that catalytic hydrogenolysis of the labile C-O benzylic bond was minimized. Following HPLC purification, [ 3 H]-fluoxetine was obtained in a state of high radiochemical purity (98%) and specific activity (20.4 Ci/mmol). The 14 C-label was introduced in the final step via a nucleophilic aromatic substitution reaction between the sodium salt of α-(2-(methylamino)ethyl)benzenemethanol and uniformly ring-labeled p-chlorobenzotrifluoride. Following purification by flash chromatography, [ 14 C]-fluoxetine was obtained in 98.3% radiochemical purity with a specific activity of 5.52 mCi/mmol. (author)

7-Diethylamino-2-oxo-2H-chromene-3-carbohydrazide

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Li-Jun Zhang

2011-05-01

Full Text Available The asymmetric unit of the title compound, C14H17N3O3, contains two independent molecules with different conformations of the ethyl groups. In the crystal, intermolecular N—H...O hydrogen bonds link the molecules into ribbons extending along the a axis.

(E-1-(3-Bromophenyl-3-(3-fluorophenylprop-2-en-1-one

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S. Rajendraprasad

2017-03-01

Full Text Available In the title compound, C15H10BrFO, the olefinic double bond adopts an E conformation. The molecule is non-planar as seen by the dihedral angle of 48.92 (11° between the bromophenyl and fluorophenyl rings. The carbonyl group is twisted from the plane of the bromophenyl ring and the olefinic double bond. The trans conformation of the C=C double bond in the central enone group is confirmed by the C—C=C—C torsion angle of −165.7 (2°.

meso-4,4′-Difluoro-2,2′-{[(3aR,7aS-2,3,3a,4,5,6,7,7a-octahydro-1H-1,3-benzimidazole-1,3-diyl]bis(methylene}diphenol

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Augusto Rivera

2013-02-01

Full Text Available In the crystal structure of the title compound, C21H24F2N2O2, there are two intramolecular O—H...N hydrogen bonds involving the N atoms of the imidazolidine ring and the hydroxy groups. The crystal studied was a meso compound obtained by the reaction of the aminal (2S,7R,11S,16R-1,8,10,17-tetraazapentacyclo[8.8.1.18,17.02,7.011,16]cosane with 4-fluorophenol. The imidazolidine ring has a twisted conformation with a CH—CH—N—CH2 torsion angle of 44.99 (14° and, surprisingly, the lone pairs of the N atoms are disposed in a syn isomerism, making the title compound an exception to the typical `rabbit-ear effect' in 1,2-diamines. In the crystal, molecules are linked via C—H...F hydrogen bonds, forming chains along the c-axis direction. These chains are linked via another C—H...F hydrogen bond, forming a three-dimensional network.

15-00368_SI_NP.docx

Indian Academy of Sciences (India)

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Figure S1. The correlation graphs between calculated and observed geometrical parameters of the studied compound. Figure S2. 1H NMR of the title compound. Figure S3. 13C NMR of the title compound. Figure S4. IR of the title compound. Table S1. Hydrogen bonding information (Å, °) of the title compound. Table S2.

3-Methyl-4-(3-methylphenyl-5-(2-pyridyl-4H-1,2,4-triazole

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Dun-Ru Zhu

2009-05-01

Full Text Available In the molecule of the title compound, C15H14N4, the triazole ring is oriented at dihedral angles of 30.8 (2 and 67.4 (2° with respect to the pyridine and benzene rings, respectively. The crystal structure is stabilized by C—H...N hydrogen-bonding interactions, forming chains of molecules along [overline{1}01].

1,3,5-Tri-p-tolylpentane-1,5-diol

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A. Thiruvalluvar

2014-02-01

Full Text Available In the title compound, C26H30O2, the central benzene ring forms dihedral angles of 14.85 (15 and 28.17 (14° with the terminal benzene rings. The dihedral angle between the terminal benzene rings is 32.14 (13°. The crystal packing exhibits two strong intermolecular O—H...O hydrogen bonds, forming directed four-membered co-operative rings. A region of disordered electron density, most probably disordered ethyl acetate solvent molecules, occupying voids of ca 519 Å3 for an electron count of 59, was treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. Their formula mass and unit-cell characteristics were not taken into account during refinement. The structure was refined as an inversion twin [absolute structure parameter = −0.3 (4].

Double labeling autoradiography. Cell kinetic studies with 3H- and 14C-thymidine

International Nuclear Information System (INIS)

Schultze, B.

1981-01-01

Examples of the multiple applicability of the double labeling method with 3 H- and 14 C-TdR are demonstrated. Double labeling with 3 H- and 14 C-TdR makes it possible to determine the cycle and its phases with high precision by modifying the usual percent labeled mitoses method with a single injection of 3 H-TdR. In addition, data is provided on the variances of the transit times through the cycle phases. For example, in the case of the jejunal crypt cells of the mouse, the transit times through successive cycle phases are uncorrelated. In the case of glial cells the double labeling method provides cell kinetic parameters despite the paucity of proliferating glial cells. In the adult untreated animal, glial cell mitoses are so rare that the percent labeled mitoses method can not be utilized. However, the S-phase duration can be measured by double labeling and the cycle time can be determined by the so-called method of labeled S phases. With the latter method the passage through the S phase of the 3 H-TdR-labeled S phase cells can be registered by injecting 14 C-TdR at different time intervals following 3 H-TdR application. In this way an S-phase duration of about 10 hr and a cycle time of about 20 hr was found for glial cells in the adult untreated mouse. An exchange of glial cells between the growth fraction and the nongrowth fraction has also been shown by double labeling. A quite different application of the double labeling method with 3H- and 14 C-TdR is the in vivo study of the cell cycle phase-specific effect of drugs used in chemotherapy of tumors. The effect of vincristine on these cells has been studied. Vincristine affects cells in S and G2 in such a manner that they are arrested during the next metaphase and subsequently become necrotic. It has no effect on G1 cells

Crystal structure of 5-[bis(methylsulfonylmethyl]-1,3-dimethyl-5-(methylsulfonylpyrimidine-2,4,6(1H,3H,5H-trione

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Eyad Mallah

2015-01-01

Full Text Available In the title compound, C10H16N2O9S3, the pyrimidine ring of the 1,3-dimethyl barbituric acid moiety has an envelope conformation with the C atom carrying the methylsulfonyl and bis(methylsulfonylmethyl substituents as the flap. The dihedral angle between mean plane of the pyrimidine ring and the S/C/S plane is 72.4 (3°. In the crystal, molecules are linked via C—H...O hydrogen bonds, forming a three-dimensional structure.

1-(3-Methoxyphenyl-2-(phenylsulfonylethan-1-one

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Sammer Yousuf

2012-08-01

Full Text Available In the title compound, C15H14O4S, the dihedral angle between the benzene and phenyl rings is 88.74 (10°. In the crystal, molecules are linked into a three-dimensional network by C—H...O hydrogen bonds and π–π stacking interactions [centroid–centroid distances = 3.6092 (13–3.8651 (13 Å].

Synthesis of /sup 14/C- and /sup 3/H-labelled 4-(4-nitrophenyl)aminophenylisothiocyanate (Go 9333/CGP 4540; amoscanate)

Energy Technology Data Exchange (ETDEWEB)

Anjaneyulu, B.; Maller, R.K.; Nagarajan, K. (Hindustan Ciba-Geigy Ltd., Bombay (India). Isotope Lab.); Kueng, W.; Wirz, B. (Ciba-Geigy A.G., Basel (Switzerland))

1985-04-01

Amoscanate, a broad spectrum anthelmintic, labelled with carbon-14 on the isothiocyanate carbon atom was prepared in an overall yield of 13% at a specific activity of 4.13 ..mu..Ci/mg from potassium (/sup 14/C)thiocyanate. The 4-nitro(U-/sup 14/C)phenyl ring labelled compound was synthesized in 20.4% overall yield from (U-/sup 14/C)aniline at a specific activity of 12.2 ..mu..Ci/mg. The corresponding tritiated compound was prepared from 4-amino(2-/sup 3/H)acetanilide at 112 ..mu..Ci/mg. Labelling with tritium in the aromatic ring bearing the isothiocyanate group was achieved by catalysed halogen-tritium replacement. However, for pharmacokinetic and metabolism studies in experimental animals, the /sup 14/C- and /sup 3/H-labels associated with the phenylisothiocyanate moiety subsequently proved disadvantageous because of the instability of the labels in vivo.

2-Benzyl-6-chloro-1-(4-methylphenyl-1H-indole-3-carbonitrile

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Qiao Yan

2011-12-01

Full Text Available In the title compound, C23H17ClN2, the dihedral angle between the indole ring and the attached tolyl ring is 86.97 (8°. Weak C—H...N(nitrile hydrogen bonding, and C—H...π(aromatic and short Cl...π(aromatic [3.628 (1 Å] interactions consolidate the crystal packing.

2,6-Diphenyl-4-(2-thienyl-1,4-dihydropyridine-3,5-dicarbonitrile

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Xiao-Tong Zhu

2009-09-01

Full Text Available The asymmetric unit of the title compound, C23H15N3S, contains two crystallographically independent molecules. The pyridine rings adopt envelope conformations. The thiophene rings are oriented at dihedral angles of 77.97 (4/53.53 (4 and 78.44 (4/57.11 (4° with respect to the phenyl rings, while the dihedral angles between the phenyl rings are 48.51 (4 and 44.49 (4°. In the crystal structure, intermolecular N—H...N hydrogen bonds link the molecules into chains along the c axis. The S, C and H atoms of one of the thiophene rings are disordered over two orientations, with occupancy ratios of 0.314 (15:0.686 (15.

Distribution of 14C-activity among the organic acids in the Satsuma mandarin fruits fed with 14C-compounds

International Nuclear Information System (INIS)

Kubota, Shuji; Akao, Shoichiro; Hayashida, Michito.

1978-01-01

1. Twenty four hours after 14 CO 2 feeding to the leaves, malic acid had the highest level of total and specific radioactivity among the organic acids extracted from the juice vesicles, and citric acid had the second highest total activity. An unidentified acid compound had a relatively high activity. 2. Pyruvic acid-2- 14 C was fed as a substrate for acid formation to the one young fruit on a shoot, and NaH 14 CO 3 was fed as a source of carbon-dioxide to the other young fruit through the pedicel. After three hours of pyruvic acid feeding, malic acid, citric acid and aspartic acid were the major labelled compounds in the vesicles. Then, a marked increase and redistribution of activity in acids took place with time, and the levels of total and specific activity in citric acid increased steadily. The sorts of labelled compounds into which activity was incorporated from NaH 14 CO 3 were essentially similar to those in pyruvic acid-2- 14 C feeding. 3. These results seem to support the theory that the dark fixation of carbon-dioxide plays an important role in the synthesis of the organic acids in citrus fruit vesicles. (auth.)

Poly[(μ4-biphenyl-3,3′-dicarboxylatobis[μ2-1,1′-(butane-1,4-diyldiimidazole](μ2-oxalatodimanganese(II

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Bao-Yong Zhu

2010-10-01

Full Text Available In the title coordination compound, [Mn2(C14H8O4(C2O4(C10H14N42]n, the biphenyl-3,3′-dicarboxylate and oxalate anions, both situated on inversion centres, function in a bridging mode, linking the dinuclear MnII atoms into wave-like layers. Each 1,1′-(1,4-butane-1,4-diyldiimidazole ligand coordinates to two MnII atoms located in adjacent layers via Mn—N coordination bonds, giving a three-dimensional network. As the methylene groups can bend freely relative to each other due to the C atoms connected via single bonds, the 1,1′-(butane-1,4-diyldiimidazole ligand forms an S-shaped conformation, which makes the void in the three-dimensional network distorted.

2-Phenyl-7-(4-pyridylmethylamino-1,2,4-triazolo[1,5-a][1,3,5]triazin-5(4H-oneFused heterocyclic systems with s-triazine ring. Part 17. For part 16, see Dolzhenko et al. (2011.

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Lip Lin Koh

2011-01-01

Full Text Available In the title compound, C16H13N7O, the 1,2,4-triazolo[1,5-a][1,3,5]triazine heterocyclic system is essentially planar (r.m.s. deviation = 0.0375 Å. The attached benzene ring lies almost in the mean plane of 1,2,4-triazolo[1,5-a][1,3,5]triazine [dihedral angle = 1.36 (23°], while the pyridine ring is turned out of this plane by the aminomethyl bridge [dihedral angle = 69.22 (9°]. The amino group H atom is involved in intramolecular hydrogen bonding with a triazole N atom. In the crystal, molecules are connected via C(=ONH...N hydrogen bonds into C(11 chains parallel to [100]. The amino group H atom acts as a hydrogen-bond donor, forming an NH...O=C hydrogen bond with the carbonyl O atom, which links the molecules into C(6 chains running along [011] and [01overline{1}].

Crystal structures of bis[(9S,13S,14S-3-methoxy-17-methylmorphinanium] tetrachloridocobaltate and tetrachloridocuprate

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Eric Gauchat

2017-01-01

Full Text Available (9S,13S,14S-3-Methoxy-17-methylmorphinan (dextromethorphan forms two isostructural salts with (a tetrachloridocobaltate, namely bis[(9S,13S,14S-3-methoxy-17-methylmorphinanium] tetrachloridocobaltate, (C18H26NO2[CoCl4], and (b tetrachloridocuprate, namely bis[(9S,13S,14S-3-methoxy-17-methylmorphinanium] tetrachloridocuprate, (C18H26NO2[CuCl4]. The distorted tetrahedral anions are located on twofold rotational axes. The dextromethorphan cation can be described as being composed of two ring systems, a tetrahydronaphthalene system A+B and a decahydroisoquinolinium subunit C+D, that are nearly perpendicular to one another: the angle between mean planes of the A+B and C+D moieties is 78.8 (1° for (a and 79.0 (1° for (b. Two symmetry-related cations of protonated dextromethorphan are connected to the tetrachloridocobaltate (or tetrachloridocuprate anions via strong N—H...Cl hydrogen bonds, forming neutral ion associates. These associates are packed in the (001 plane with no strong attractive bonding between them. Both compounds are attractive crystalline forms for unambiguous identification of the dextromethorphan and, presumably, of its optical isomer, levomethorphan.

4-{[(1-Phenyl-1H-pyrazol-3-yloxy]methyl}-1,3-dioxolan-2-one

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Algirdas Šačkus

2012-11-01

Full Text Available The title compound was obtained by the reaction of tosylated glycerol carbonate with 1-phenyl-1H-pyrazol-3-ol in a good 71% yield. Detailed spectroscopic data (1H-NMR, 13C-NMR, 15N-NMR, IR, MS are presented.

(2E-3-(3-Methoxy-1-phenyl-1H-pyrazol-4-yl-2-propenal

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Algirdas Šačkus

2009-12-01

Full Text Available The palladium-catalyzed reaction of 4-bromo-3-methoxy-1-phenyl-1H-pyrazole with acrolein diethyl acetal gives the title compound in good yield. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.

Assessment of off-stoichiometric Zr33-xFe52+xSi15 C14 Laves phase compounds as permanent magnet materials

Science.gov (United States)

Gabay, A. M.; Hadjipanayis, G. C.

2018-05-01

Recently, Fe-based rare-earth-free compounds with non-cubic crystal structures were proposed as a base for permanent magnets which would not rely on critical elements. In this work, two series of alloys, Zr27Fe73-wSiw (0 ≤ w ≤ 15) and Zr33-xFe52+xSi15 (0 ≤ x ≤ 11), were prepared and characterized after annealing at 1538 K in order to determine the fundamental magnetic properties of the C36 and C14 hexagonal Laves phase compounds. A mixture of the cubic C15 and Zr6Fe23 structures was observed instead of the expected C36 structure. The hexagonal C14 was found in all Zr33-xFe52+xSi15 alloys with its lattice parameters linearly decreasing as the Fe(Si) atoms occupy the Zr sites in the Laves phase crystal structure. The solubility limit of Fe in the C14 structure at 1538 K corresponds to x = 9.5. The Curie temperature of the C14 compounds increases with deviation from the Laves phase stoichiometry from 290 K to 530 K. The room-temperature spontaneous magnetization also increases reaching, after correcting for the non-magnetic impurities, a value of 6.7 kG. The magnetocrystalline anisotropy of the off-stoichiometric C14 Laves phase was found to be uniaxial with the easy magnetization direction parallel to the hexagonal axis. Unfortunately, the anisotropy field, which does not exceed 10 kOe, is not sufficiently high to make the compounds interesting as permanent magnet materials.

Ethyl (E)-2-(2,7-dimethyl-5-oxo-4H,5H-pyrano[4,3-b]pyran-4-ylidene)acetate

OpenAIRE

Oulemda Bassou; Hakima Chicha; Latifa Bouissane; El Mostapha Rakib; Mohamed Saadi; Lahcen El Ammari

2017-01-01

In the title compound, C14H14O5, the two heterocyclic rings are coplanar (r.m.s. deviation = 0.008 Å), with the largest deviation from the mean plane being 0.012 (1) Å. The mean plane through the acetate group is inclined slightly with respect to the oxopyrano[4,3-b]pyran-4-yl system, as indicated by the dihedral angle of 1.70 (7)° between them. Two intramolecular hydrogen bonds, completing S(6) ring motifs, are observed in the molecule. In the crystal, molecules are linked by weak C—H...O hy...

The crystal structure of zwitterionic 2-{[(4-iminiumyl-3-methyl-1,4-dihydropyridin-1-ylmethyl]carbamoyl}benzoate hemihydrate

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C. S. Chidan Kumar

2017-07-01

Full Text Available The asymmetric unit of the title compound, C15H15N3O3·0.5H2O, comprises two 2-{[(4-iminiumyl-3-methyl-1,4-dihydropyridin-1-ylmethyl]carbamoyl}benzoate zwitterions (A and B and a water molecule. The dihedral angles between the pyridine and phenyl rings in the zwitterions are 53.69 (10 and 73.56 (11° in A and B, respectively. In the crystal, molecules are linked by N—H...O, O—H...O, C—H...O and C—H...π(ring hydrogen bonds into a three-dimensional network. The crystal structure also features π–π interactions involving the centroids of the pyridine and phenyl rings [centroid–centroid distances = 3.5618 (12 Å in A and 3.8182 (14 Å in B].

Synthesis, characterization, crystal structure, and thermal analysis of 2-chloro-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl) acetamide

Energy Technology Data Exchange (ETDEWEB)

Sharma, R. [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics & Electronics (India); Nayak, P. S.; Narayana, B. [Mangalore University, Mangalagangotri, Department of Studies in Chemistry (India); Kant, R., E-mail: rkvk.paper11@gmail.com [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics & Electronics (India)

2015-12-15

The title compound, C{sub 13}H{sub 14}O{sub 2}N{sub 3}Cl, has been synthesized by the reaction of chloroacetyl chloride with 4-aminoantipyrine in basic media and characterized by FT-IR, CHN elemental analysis, UV-Vis, TGA, DTA, DSC and single crystal X-ray diffraction. crystals are monoclinic, sp. gr. P2{sub 1}/c, a = 6.9994(6), b = 12.4035(13), c = 15.836(2) Å, β = 100.367(9)°, Z = 4. The crystal structure is stabilized by N–H···O and C–H···O interactions, the former interactions result in the formation of dimers corresponding to R{sub 2}{sup 2} (10) graphset motif and the dimers are further connected by C–H···O hydrogen bonding forming chains. In addition, the thermal stability of the compound was determined by TGA, DTA, DSC analysis, and absorption at λ{sub max} = 298 nm was determined by UV-Vis spectrophotometer.

Crystal structures of 2-methoxyisoindoline-1,3-dione, 1,3-dioxoisoindolin-2-yl methyl carbonate and 1,3-dioxo-2,3-dihydro-1H-benzo[de]isoquinolin-2-yl methyl carbonate: three anticonvulsant compounds

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Fortune Ezemobi

2014-12-01

Full Text Available The title compounds, C9H7NO3, (1, C10H7NO5, (2, and C14H9NO5, (3, are three potentially anticonvulsant compounds. Compounds (1 and (2 are isoindoline derivatives and (3 is an isoquinoline derivative. Compounds (2 and (3 crystallize with two independent molecules (A and B in their asymmetric units. In all three cases, the isoindoline and benzoisoquinoline moieties are planar [r.m.s. deviations are 0.021 Å for (1, 0.04 and 0.018 Å for (2, and 0.033 and 0.041 Å for (3]. The substituents attached to the N atom are almost perpendicular to the mean planes of the heterocycles, with dihedral angles of 89.7 (3° for the N—O—Cmethyl group in (1, 71.01 (4 and 80.00 (4° for the N—O—C(=OO—Cmethyl groups in (2, and 75.62 (14 and 74.13 (4° for the same groups in (3. In the crystal of (1, there are unusual intermolecular C=O...C contacts of 2.794 (1 and 2.873 (1 Å present in molecules A and B, respectively. There are also C—H...O hydrogen bonds and π–π interactions [inter-centroid distance = 3.407 (3 Å] present, forming slabs lying parallel to (001. In the crystal of (2, the A and B molecules are linked by C—H...O hydrogen bonds, forming slabs parallel to (10-1, which are in turn linked via a number of π–π interactions [the most significant centroid–centroid distances are 3.4202 (7 and 3.5445 (7 Å], forming a three-dimensional structure. In the crystal of (3, the A and B molecules are linked via C—H...O hydrogen bonds, forming a three-dimensional structure, which is consolidated by π–π interactions [the most significant inter-centroid distances are 3.575 (3 and 3.578 (3 Å].

2-Methyl-1,10b-dihydro-5H-pyrazolo[1,5-c][1,3]benzoxazin-5-one

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Jan Světlík

2009-05-01

Full Text Available In the title compound, C11H10N2O2, a potential inhibitor of the cyclooxygenase-2 isoenzyme, the pyrazoline ring exists in a flat-envelope conformation while the puckering of the central oxazine ring is more severe. As a result, the molecule as a whole is non-planar. The formal sp3 pyrazoline N atom is sp2 hybridized, with the lone-pair electrons delocalized through conjugation with the carbonyl group rather than the double bond of the pyrazoline ring.

(E-6-Amino-1,3-dimethyl-5-[(pyridin-2-ylmethylideneamino]pyrimidine-2,4(1H,3H-dione

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Irvin Booysen

2011-09-01

Full Text Available In the title compound, C12H13N5O2, a Schiff-base-derived chelate ligand, the non-aromatic heterocycle and its substituents essentially occupy one common plane (r.m.s. of fitted non-H atoms = 0.0503 Å. The N=C bond is E-configured. Intracyclic angles in the pyridine moiety cover the range 117.6 (2–124.1 (2°. Intra- and intermolecular N—H...N and N—H...O hydrogen bonds are observed in the crystal structure, as are intra- and intermolecular C—H...O contacts which, in total, connect the molecules into a three-dimensional network. The shortest ring-centroid-to-ring-centroid distance of 3.5831 (14 Å is between the two different types of six-membered rings.

Synthesis of pinacolyl [14C]methylphosphonochloridate

International Nuclear Information System (INIS)

Horvat, J.; Keglevic, D.; Klaic, B.; Kveder, S.; Ladesic, B.; Cosic, M.; Zupanc, S.

1982-01-01

A three-step synthetic route to pinacolyl [ 14 C]methylphosphonochloridate (3) from [ 14 C]methyl iodide is described. Condensation of sodium di-n-butyl phosphite with [ 14 C]methyl iodide gave di-n-butyl [ 14 C]methylphosphonate (1) which was converted into [ 14 C]methylphosphonic dichloride (2) by prolonged refluxing with thionyl chloride. Reaction of 2 with pinacolyl alcohol in the presence of N,N-di-n--propylaniline as the base afforded the title compound 3. The radiochemical yield of redistilled 3 was 34,2% based on 1, and the overall radiochemical yield was 20,0% from [ 14 C]methyl iodide. (author)

Incineration of radioactive wastes containing only C-14 and H-3

International Nuclear Information System (INIS)

Garcia, Corazon M.

1992-01-01

C-14 and H-3 arc popularly used in chemical and biological research institutions in the Philippines. Most of the solid radioactive wastes generated by these institutions consist of combustible materials such as paper and accumulated environmental samples. Liquid wastes usually contain organic substances. The method proposed for managing C-14 and H-3 wastes is incineration which is expected to provide an acceptable means of disposal for C-14 and H-3 and their hazardous organic constituent. In the incineration process) the radioactively contaminated waste will be mixed with non-radioactive combustible wastes to lower the activity concentration and to improve the efficiency of combustion which will be carried out in a locally fabricated drum incinerator. The calculations presented determines the concentration limit for the incinerable wastes and the restriction on specific activity of the particles of the incinerable wastes containing C-14 or H-3 on the basis of the accepted air concentration and on the annual dose limit for an average radiation worker in the country. In the calculations for C-14, considerations were taken on the exposure received from the deposition of radioactive particles in the lungs containing unoxidized carbon. Calculations for H-3, however, is based on the assumption that the concentration of the radionuclide in the body water is the same as that in the environment. (author)

17 CFR 402.2d - Appendix D-Modification of § 240.15c3-1d of this title, relating to satisfactory subordination...

Science.gov (United States)

2010-04-01

... 17 Commodity and Securities Exchanges 3 2010-04-01 2010-04-01 false Appendix D-Modification of § 240.15c3-1d of this title, relating to satisfactory subordination agreements, for purposes of § 402.2...—Modification of § 240.15c3-1d of this title, relating to satisfactory subordination agreements, for purposes of...

Environmental 14C and 3H activities: global trends and local contamination

International Nuclear Information System (INIS)

Krajcar Bronic, I.; Obelic, B.; Horvatincic, N.

2000-01-01

The anthropogenic disturbance of natural distributions of radiocarbon ( 14 C) and tritium ( 3 H) due to the release of bomb-produced isotopes occurred after the World War II and at the same time the monitoring of these isotopes started at several stations in the world. Radioactive isotopes 14 C and 3 H, together with the stable isotopes 2 H and 18 O, are very important tracers in environmental, climatological and hydrological studies. Monitoring of environmental levels of 14 C and 3 H in Croatia started more then 20 years ago, while that of the stable isotopes somewhat later. The monitoring was performed at the three types of stations: a) 'clean-air' sites, which are supposed to reflect only the global disturbance of the atmospheric isotope concentrations, b) in a densely populated industrial center, where the effect of intense fossil-fuel combustion is expected, and local contamination from institutions using radioactive-labeled material is also possible, and c) at locations around the Nuclear Power Plant Krsko. The mean yearly 3 H activities in precipitation continuously decrease since the beginning of monitoring approaching slowly the natural equilibrium. The monthly 3 H activities show seasonal variations, with maximum in early summer and minimum in early winter. Both seasonal variations and the decrease of the mean yearly values are typical for continental stations of the Northern Hemisphere. At the sampling site located at the Institute, several periods of higher 3 H activities were observed, due to the local contamination with the tritium-labeled material. The 14 C concentration in the atmosphere shows also the continuous decrease of the mean yearly values and superposed seasonal fluctuations, with higher activity during summer. Seasonal peak-to-peak variations are higher in the area of the city of Zagreb than at the clean-air site on the mountain (about 1000 m a.s.l.). This difference is caused by the introduction of CO 2 (containing no 14 C isotope

Crystal structure and thermochemical properties of 1-decylammonium hydrobromide (C10H21NH3Br)(s)

International Nuclear Information System (INIS)

Zhang Lijun; Di Youying; Lu Dongfei

2011-01-01

Highlights: → Crystal structure of 1-decylammonium hydrobromide was reported. → Lattice potential energy of the compound was obtained. → Molar volumes of the compound and its cation were obtained. → Ionic radius of its cation of the compound was calculated. → Molar enthalpy of dissolution at infinite dilution was determined. → Hydration enthalpies of the compound and its cation were calculated. - Abstract: The crystal structure of 1-decylammonium hydrobromide was determined by X-ray crystallography. Lattice potential energy and molar volumes of the solid compound and its cation were obtained respectively. The ionic radius of the cation can be calculated from the corresponding effective volume of the cation. The molar enthalpies of dissolution of the compound at different concentrations m/(mol . kg -1 ) at T = 298.15 K were measured by an isoperibol solution-reaction calorimeter at T = 298.15 K. According to the Pitzer's electrolyte solution theory, the molar enthalpy of dissolution of the compound at infinite dilution (Δ s H m ∞ ) and Pitzer parameters (β MX (0)L and β MX (1)L ) were obtained. The values of apparent relative molar enthalpies ( Φ L) of the title compound and relative partial molar enthalpies (L 2 -bar and L 1 -bar) of the solute and the solvent at different concentrations were derived from the experimental values of the enthalpy of dissolution of the compound. Finally, hydration enthalpies of the compound and its cation were calculated by designing a thermochemical cycle in accordance with lattice potential energy and the molar enthalpy of dissolution of the title compound at infinite dilution.

Synthesis of /sup 14/C- and /sup 3/H-labeled fluoxetine, a selective serotonin uptake inhibitor

Energy Technology Data Exchange (ETDEWEB)

Robertson, D.W.; Krushinski, J.H.; Wong, D.T.; Kau, D.

1987-11-01

Fluoxetine (N-methyl-..gamma..-(4-(trifluoromethyl)phenoxy) benzenepropanamine) is a potent, highly selective serotonin uptake inhibitor that is useful in treating a variety of major psychiatric derangements. We have synthesized this compound in /sup 14/C- and /sup 3/H-labeled forms. The tritium label was introduced in the final step by catalytic dehalogenation of the brominated fluoxetine precursor. Reaction conditions could be controlled such that catalytic hydrogenolysis of the labile C-O benzylic bond was minimized. Following HPLC purification, (/sup 3/H)-fluoxetine was obtained in a state of high radiochemical purity (98%) and specific activity (20.4 Ci/mmol). The /sup 14/C-label was introduced in the final step via a nucleophilic aromatic substitution reaction between the sodium salt of ..cap alpha..-(2-(methylamino)ethyl)benzenemethanol and uniformly ring-labeled p-chlorobenzotrifluoride. Following purification by flash chromatography, (/sup 14/C)-fluoxetine was obtained in 98.3% radiochemical purity with a specific activity of 5.52 mCi/mmol.

Syntheses, crystal structures, and properties of the isotypic pair [Cr(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O and [In(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O

Energy Technology Data Exchange (ETDEWEB)

Van, Nguyen-Duc; Kleeberg, Fabian M.; Schleid, Thomas [Institut fuer Anorganische Chemie, Universitaet Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart (Germany)

2015-11-15

Single crystals of [Cr(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O and [In(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O were obtained by reactions of aqueous solutions of the acid (H{sub 3}O){sub 2}[B{sub 12}H{sub 12}] with chromium(III) hydroxide and indium metal shot, respectively. The title compounds crystallize isotypically in the trigonal system with space group R anti 3c (a = 1157.62(3), c = 6730.48(9) pm for the chromium, a = 1171.71(3), c = 6740.04(9) pm for the indium compound, Z = 6). The arrangement of the quasi-icosahedral [B{sub 12}H{sub 12}]{sup 2-} dianions can be considered as stacking of two times nine layers with the sequence..ABCCABBCA.. and the metal trications arrange in a cubic closest packed..abc.. stacking sequence. The metal trications are octahedrally coordinated by six water molecules of hydration, while another fifteen H{sub 2}O molecules fill up the structures as zeolitic crystal water or second-sphere hydrating species. Between these free and the metal-bonded water molecules, bridging hydrogen bonds are found. Furthermore, there is also evidence of hydrogen bonding between the anionic [B{sub 12}H{sub 12}]{sup 2-} clusters and the free zeolitic water molecules according to B-H{sup δ-}..{sup δ+}H-O interactions. Vibrational spectroscopy studies prove the presence of these hydrogen bonds and also show slight distortions of the dodecahydro-closo-dodecaborate anions from their ideal icosahedral symmetry (I{sub h}). Thermal decomposition studies for the example of [Cr(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O gave no hints for just a simple multi-stepwise dehydration process. (Copyright copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

N-(2-Methylphenyl-1,2-benzoselenazol-3(2H-one

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Xu Zhu

2013-10-01

Full Text Available In the title Ebselen [systematic name: (2-phenyl-1,2-benzoisoselenazol-3-(2H-one] analogue, C14H11NOSe, the benzisoselenazolyl moiety (r.m.s. deviation = 0.0209 Å is nearly perpendicular to the N-arenyl ring, making a dihedral angle of 78.15 (11°. In the crystal, molecules are linked by C—H...O and Se...O interactions into chains along the c-axis direction. The Se...O distance [2.733 (3 Å] is longer than that in Ebselen (2.571 (3 Å].

Radioactive levels and doses of 3H and 14C in white spirits

International Nuclear Information System (INIS)

Deng, G.

1992-01-01

'Full Text:' White (and yeast) spirits is a general name for strong alcoholic beverages in China. The paper reports levels and doses of 3 H and 14 C in 65 spirits samples between 1986 and 1987. Experiments were made by measuring end analyzing each sample, using a low background liquid scintillation spectrometer. Radioactive levels of 65 spirits samples are as follows: Variant range of 3 H activity is 98.2 - 170.6Bq.dm -3 and its average is 149.2 ± 17.3Bq.dm -3 ; Variant range of 14 C activity is 38.8-80.2Bq.dm -3 and its average is 57.4±8.2Bq.dm -3 . If the man drinks 200cm 3 of spirits daily, the annual dose equivalents will be 0.19uSv of 3 H and 2.5uSv of 14 C . In ordinary strong alcoholic beverages that contain 57-60% alcohol, the mean 3 H and 14 C activities are 153.8Bq.dm -3 and 60.3Bq.dm -3 , respectively, but in spirits of lower alcoholic content (38-40%), the mean 3H activity is 114.6Bq.dm -3 , that is 25.5% less than ordinary spirits, and the mean 14 C activity is 46.1Bq.dm -3 , that is 23.5% less than ordinary spirits. We compared the 3 H and 14 C contents of five kinds of staple grains from both Sichuan and Guangdong provinces. We learned that the level of activity in spirits is ten times higher than in grains and water, and the level of 14 C activity in spirits is equivalent to that in grains. White spirits has fully concentrated 3 H and 14 C from both grain and water, and activities increase with increasing alcoholic content. 3 H in spirits probably is averaged from both water and grain, and 14 C is averaged mostly from grain. (author)

Crystal structure of N′-[(E-(1S,3R-(3-isopropyl-1-methyl-2-oxocyclopentylmethylidene]-4-methylbenzenesulfonohydrazide

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David Tymann

2015-12-01

Full Text Available The title compound, C17H24N2O3S, was synthesized in order to determine the relative configuration of the corresponding β-keto aldehyde. In the U-shaped molecule, the five-membered ring approximates an envelope, with the methylene C atom adjacent to the quaternary C atom being the flap, and the methyl and isopropyl substituents lying to the same side of the ring. The dihedral angles between the four nearly coplanar atoms of the five-membered ring and the flap and the aromatic ring are 35.74 (15 and 55.72 (9°, respectively. The bond angles around the S atom are in the range from 103.26 (12 to 120.65 (14°. In the crystal, molecules are linked via N—H...O hydrogen bonds, forming a chain along the a axis.

14C2H4: distribution of 14C-labeled tissue metabolites in pea seedlings

International Nuclear Information System (INIS)

Giaquinta, R.; Beyer, E. Jr.

1977-01-01

The 14 C-metabolite distribution pattern following 14 C 2 H 4 metabolism in intact pea seedlings (Pisum sativum L.) was determined under various conditions. After a 24 hr exposure to 14 C 2 H 4 , the majority of 14 C-metabolites were water-soluble (60-70%) with lesser amounts in the protein (10-15%), lipid (1%), and insoluble (1-2%) fractions. Ion exchange chromatography of the water-soluble components into basic, neutral, and acidic fractions revealed a 50:40:10 distribution, respectively. Chromatography of the neutral fraction revealed two regions of radioactivity (Rf=0.38) and 0.63 which did not cochromatograph with twenty-two known sugars or neutral metabolites. Chromatograms of the basic fraction contained 3 regions of radioactivity. Similar distribution patterns were noted when 14 C 2 H 4 exposure was followed by a 6 hr air chase or when 5% CO 2 , an antagonist of ethylene action, was present during the exposure. Marked differences in the 14 C-metabolite distribution patterns were obtained when 14 CO 2 was substituted for 14 C 2 H 4 . These results indicate that the metabolic pathway involved in ethylene metabolism is different from that involved in intermediately carbon metabolism. (auth.)

Production of 15N-enriched nitric acid (H15NO3

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C. R. Sant Ana Filho

2008-12-01

Full Text Available Techniques that employ 15N have proved to be an important tool in many areas of the agronomic and biomedical sciences. Nevertheless, their use is limited by methodological difficulties and by the price of compounds in the international market. Nitric compounds (15NO3- have attracted the interest of researchers. However, these compounds are not currently produced in Brazil. Thus, in the present work H15NO3 was obtained from the oxidation of anhydrous 15NH3. The method we used differs from the industrial process in that the absorption tower is replaced with a polytetrafluoroethylene-lined, stainless-steel hydration reactor. The process output was evaluated based on the following parameters: reaction temperature; ratio of reagents; pressure and flow of 15NH3(g through the catalyst (Pt/Rh. The results showed that, at the best conditions (500 ºC; 50 % excess O2; 0.4 MPa; and 3.39 g.min-1 of 15NH3, a conversion percentage (N-15NH3 to N-15NO3- of 62.2 %, an overall nitrogen balance (N-15NH3 + N-15NO3- of 86.8 %, and purity higher than 99 % could be obtained.

(2-Methyl-4-oxo-4H-pyran-3-olato-κ2O3,O4bis(triphenylphosphane-κPcopper(I–triphenylphosphane–methanol (1/1/1

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Fabian M. A. Muller

2011-05-01

Full Text Available In the title compound, [Cu(C6H5O3(C18H15P2]·C18H15P·CH3OH, the pyran-4-one ring is appromimately planar (r.m.s deviation = 0.0138 Å, with the CuI atom 0.451 (5 Å out of the plane. The CuI atom has a distorted tetrahedral coordination. The O—Cu—O angle is 80.07 (8° and the P—Cu—P angle is 123.49 (3°. The crystal packing is stablized by intramolecular C—H...O interactions and intermolecular C—H...O and O—H...O interactions.

Solvothermal synthesis and characterisation of new one-dimensional indium and gallium sulphides: [C1N4H26]0.5[InS2] and [C1N4H26]0.5[GaS2

International Nuclear Information System (INIS)

Vaqueiro, Paz

2006-01-01

Two new main group metal sulphides, [C 1 N 4 H 26 ] 0.5 [InS 2 ] (1) and [C 1 N 4 H 26 ] 0.5 [GaS 2 ] (2) have been prepared solvothermally in the presence of 1,4-bis(3-aminopropyl)piperazine and their crystal structures determined by single-crystal X-ray diffraction. Both compounds are isostructural and crystallise in the monoclinic space group P2 1 /n (Z=4), with a=6.5628(5), b=11.2008(9), c=12.6611(9) A and β=94.410(4) o (wR=0.035) for compound (1) and a=6.1094(5), b=11.2469(9), c=12.7064(10) A and β=94.313(4) o (wR=0.021) for compound (2). The structure of [C 1 N 4 H 26 ] 0.5 [MS 2 ] (M=In,Ga) consists of one-dimensional [MS 2 ] - chains which run parallel to the crystallographic a axis and are separated by diprotonated amine molecules. These materials represent the first example of solvothermally prepared one-dimensional gallium and indium sulphides. -- Graphical abstract: [C 1 N 4 H 26 ] 0.5 [InS 2 ] and [C 1 N 4 H 26 ] 0.5 [GaS 2 ], prepared under solvothermal conditions, consist of one-dimensional [MS 2 ] - chains separated by diprotonated 1,4-bis(3-aminopropyl)piperazine molecules

The radioactivity estimation of 14C and 3H in graphite waste samples of the KRR-2.

Science.gov (United States)

Reyoung Kim, Hee

2013-09-01

The radioactivity of (14)C and (3)H in graphite samples from the dismantled Korea Research Reactor-2 (the KRR-2) site was analyzed by high-temperature oxidation and liquid scintillation counting, and the graphite waste was suggested to be disposed of as a low-level radioactive waste. The graphite samples were oxidized at a high temperature of 800 °C, and their counting rates were measured by using a liquid scintillation counter (LSC). The combustion ratio of the graphite was about 99% on the sample with a maximum weight of 1g. The recoveries from the combustion furnace were around 100% and 90% in (14)C and (3)H, respectively. The minimum detectable activity was 0.04-0.05 Bq/g for the (14)C and 0.13-0.15 Bq/g for the (3)H at the same background counting time. The activity of (14)C was higher than that of (3)H over all samples with the activity ratios of the (14)C to (3)H, (14)C/(3)H, being between 2.8 and 25. The dose calculation was carried out from its radioactivity analysis results. The dose estimation gave a higher annual dose than the domestic legal limit for a clearance. It was thought that the sampled graphite waste from the dismantled research reactor was not available for reuse or recycling and should be monitored as low-level radioactive waste. Copyright © 2013 Elsevier Ltd. All rights reserved.

Ethyl 4-oxo-2,3,4,9-tetrahydro-1H-carbazole-3-carboxylate

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Cevher Gündoğdu

2011-06-01

Full Text Available In the title compound, C15H15NO3, the carbazole skeleton includes an ethoxycarbonyl group at the 3-position. In the indole ring system, the benzene and pyrrole rings are nearly coplanar, forming a dihedral angle of 0.89 (4°. The cyclohexenone ring has an envelope conformation. In the crystal, intermolecular N—H...O and C—H...O hydrogen bonds link the molecules into a three dimensional network. A weak C—H...π interaction is also observed.

Butane-1,4-diammonium bis(pyridine-2,6-dicarboxylato-κ3O2,N,O6cadmate(II dihydrate

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Najmeh Firoozi

2008-10-01

Full Text Available In the title compound, (C4H14N2[Cd(C7H3NO42]·2H2O, the CdII ion is coordinated by four O atoms [Cd—O = 2.2399 (17–2.2493 (17 Å] and two N atoms [Cd—N = 2.3113 (15 and 2.3917 (15 Å] from two tridentate pyridine-2,6-dicarboxylato ligands in a distorted octahedral geometry. The uncoordinated water molecules are involved in O—H...O and N—H...O hydrogen bonds, which contribute to the formation of a three-dimensional supramolecular structure, along with π–π stacking interactions [centroid–centroid distances of 3.5313 (13 and 3.6028 (11 Å between the pyridine rings of neighbouring dianions].

Uptake of [3H]PAH and [14C]urate into isolated proximal tubular segments of the pig kidney

International Nuclear Information System (INIS)

Schali, C.; Roch-Ramel, F.

1981-01-01

Segments of proximal convoluted (PCT) and proximal straight (PST) tubules of minipigs and normal-sized pigs were microdissected (without collagenase treatment) and incubated (30 min, 37 0 C, pH 7.4) in Ringer solution (under O 2 ) containing [ 3 H]PAH (3.10 -5 M) or [ 14 C]urate (9.10 -5 M) and, in inhibitor studies, probenecid, pyrazinoic acid (PZA), urate, or PAH, all at 1 mM. In both strains the uptake of [ 3 H]PAH expressed as mean T/M ratio (cpm per ml tissue water/cpm per ml incubation medium) was significantly higher (P 14 C]urate. In eight minipigs the T/M was 4.9 +/- 0.5 in 24 PCT and 2 +/- 0.2 in 25 PST. In normal-sized pigs the T/M was 3.8 +/- 0.3 in 35 PCT (five pigs) and 1.9 +/- 0.4 in eight PST (two pigs). In inhibitor studies urate significantly depressed the uptake of [ 3 H]PAH, and unlabeled PAH depressed the uptake of [ 14 C]urate. PZA significantly inhibited the uptake of [ 14 C]urate but not that of [ 3 H]PAH, whereas probenecid had a strong inhibitory efect on the uptake of both compounds. These results suggest that [ 14 C]urate and [ 3 H]PAH are transported by a transport system located mainly in the proximal convoluted tubule. These findings are in contrast in the findings are in contrast to the findings obtained in rabbits in which the transport system of PAH and urate is mainly located in the proximal part of the pars recta

The synthesis of 5'-[14C1] and 3a, 4-[13C2] labelled panadiplon (U-78875; 3-(5'-cyclopropyl-1,2,4-oxadiazol-3-yl)-5-(1-methylethyl)-imidazo-[1,5a]-quinoxalin-4(5H)-one)

International Nuclear Information System (INIS)

Ackland, M.J.; Howard, M.R.; Dring, L.G.

1993-01-01

5'-[ 14 C 1 ]Panadiplon was prepared in 3 steps starting from [ 14 C 1 ]cyclopropane carboxylic acid and 3-(5'-cyano-1,2,4-oxadiazol-3-yl)-5-(1-methylethyl)-imidazo-[1,5a] -quinoxalin-4(5H)-one. 3a, 4-[ 13 C 2 ]Panadiplon was prepared in two steps from 13 C 2 -oxalic acid and N-1-(1-methylethyl)-o-phenylenediamine. The position of labelling was confirmed by the appearance of two coupled resonances (J C-C =80.59 Hz) at 121.95 and 154.39 ppm in the assigned 13 C-NMR spectrum. (Author)

Differential blood-brain barrier permeabilities to [14C]sucrose and [3H]inulin after osmotic opening in the rat

International Nuclear Information System (INIS)

Ziylan, Y.Z.; Robinson, P.J.; Rapoport, S.I.

1983-01-01

The blood-brain barrier (B-BB) in 3-month-old rats was opened unilaterally by infusing 1.8 m L(+)arabinose in water into the internal carotid artery through a catheter in the external carotid. Two poorly penetrating uncharged test radiotracers of differing molecular weight and size, [ 14 C]sucrose (340 daltons, radius 5 A) and [ 3 H]inulin (5500 daltons, radius 15 A), were simultaneously injected i.v. in untreated rats, or rats at 1, 30, or 50 min after infusion of hypertonic arabinose solution. Evans-blue solution was injected 5 min prior to osmotic treatment as a visual indicator of barrier integrity. In regions of uninfused control brains, the [ 14 C]sucrose permeability-surface area (PA) product approximated 10(-5) s-1, whereas PA was not measurable for [ 3 H]inulin. In arabinose-infused animals, PA products on the ipsilateral hemisphere for both [ 14 C]sucrose and [ 3 H]inulin were markedly elevated 6 min after infusion, but decreased by 35 and 55 min. In nearly all regions, statistically significant differences were not found between 6-min [ 14 C]sucrose- and [ 3 H]inulin-PA values (P greater than 0.05). However, at 35 and 55 min in most regions, the PA for [ 3 H]inulin was significantly lower (P less than 0.05) than PA for [ 14 C]sucrose. The results indicated that the B-BB closed more rapidly to larger than to smaller molecules after osmotic treatment and were consistent with a pore model for osmotic B-BB opening

5-(2,5-Dioxooxolan-3-yl-8-methyl-3,3a,4,5-tetrahydro-1H-naphtho[1,2-c]furan-1,3-dione

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Y. Z. Guo

2013-02-01

Full Text Available In the title compound, C17H14O6, the dihedral angle between the two anhydride rings is 76.01 (8°while the dihedral angles between the benzene and anhydride rings are 42.60 (7 and 68.94 (7°. The cyclohexene ring of the tetrahydronaphthalene unit exhibits an envelope conformation.

Synthesis of (+)-(3R)-3-(4-fluorophenylsulfonamido)-1,2,3,4-tetrahydro-9-[5,6,7,8,12,13-u-14C]carbazoleppropanoic acid, [14C]BAY u 3405

International Nuclear Information System (INIS)

Radtke, M.; Boberg, M.; Pleiss, U.; Rosentreter, U.

1994-01-01

The title compound [ 14 C]BAY u 3405 (1) was synthesized as part of 8-step sequence. Starting from [U- 14 C]aniline hydrogensulfate the final product 1 was obtained with a specific activity of 741 MBq/mmol (20 mCi/mmol) and a radiochemical purity of > 98 % in an overall yield of 6 and 10 % depending on the method. (author)

Crystal structure, quantum mechanical investigation, IR and NMR spectroscopy of two new organic salts: (C8H12NO)·[NO3] (I) and (C8H14N4)·[ClO4]2 (II)

Science.gov (United States)

Bayar, I.; Khedhiri, L.; Soudani, S.; Lefebvre, F.; Pereira da Silva, P. S.; Ben Nasr, C.

2018-06-01

Two new organic-inorganic hybrid materials, 4-methoxybenzylammonium nitrate, (C8H12NO)·[NO3] (I), and 2-(1-piperazinyl)pyrimidinium bis(perchlorate), (C8H14N4)·[ClO4]2(II), have been synthesized by an acid/base reaction at room temperature, their structures were determined by single crystal X-ray diffraction. Compound (I) crystallizes in the orthorhombic system and Pnma space group with a = 15.7908 (7), b = 6.8032 (3), c = 8.7091 (4) Å, V = 935.60 (7) Å3 with Z = 4. Full-matrix least-squares refinement converged at R = 0.038 and wR(F2) = 0.115. Compound (II) belongs to the monoclinic system, space group P21/c with the following parameters: a = 10.798(2), b = 7.330(1), c = 21.186(2) Å, β = 120.641 (4)°, V = 1442.7 (3) Å3and Z = 4. The structure was refined to R = 0.044, wR(F2) = 0.132. In the structures of (I) and (II), the anionic and cationic entities are interconnected by hydrogen bonding contacts forming three-dimensional networks. Intermolecular interactions were investigated by Hirshfeld surfaces and the contacts of the four different chloride atoms in (II) were compared. The Molecular Electrostatic Potential (MEP) maps and the HOMO and LUMO energy gaps of both compounds were computed. The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13C, 35Cl and 15N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands.

5-Pentyl-4-phenylsulfonyl-1H-pyrazol-3-ol

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Tara Shahani

2010-06-01

Full Text Available In the title compound, C14H18N2O3S, the 1H-pyrazole ring is approximately planar, with a maximum deviation of 0.005 (1 Å. The dihedral angle formed between the 1H-pyrazole and phenyl rings is 79.09 (5°. Pairs of intermolecular N—H...O and O...H...N hydrogen bonds form dimers between neighboring molecules, generating R22(10 ring motifs. These dimers are further linked byintermolecular N—H...O and O—H...N hydrogen bonds into a two-dimensional array parallel to the ac plane. The crystal structure is also stabilized by C—H...π interactions.

Crystal structure of (1S,2S,2′R,3a′S,5R-2′-[(5-bromo-1H-indol-3-ylmethyl]-2-isopropyl-5,5′-dimethyldihydro-2′H-spiro[cyclohexane-1,6′-imidazo[1,5-b]isoxazol]-4′(5′H-one

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Siwar Ghannay

2016-08-01

Full Text Available In the title compound, C24H32BrN3O2, the six-membered cyclohexane ring adopts a chair conformation and the isoxasolidine ring adopts a twisted conformation. The molecule has five chiral centres and the absolute configuration has been determined in this analysis. The molecular structure is stabilized by weak intramolecular C—H...O and C—H...N contacts. In the crystal, molecules are linked by N—H...N and C—H...O hydrogen bonds, forming undulating sheets parallel to the bc plane.

Synthesis and characteristics of a novel 3-D organic amine oxalate: (enH2)1.5[Bi3(C2O4)6(CO2CONHCH2CH2NH3)].6.5H2O

International Nuclear Information System (INIS)

Yu Xiaohong; Zhang Hanhui; Cao Yanning; Chen Yiping; Wang Zhen

2006-01-01

A novel 3-D compound of (enH 2 ) 1.5 [Bi 3 (C 2 O 4 ) 6 (CO 2 CONHCH 2 CH 2 NH 3 )].6.5H 2 O has been hydrothermally synthesized and characterized by IR, ultraviolet-visible diffuse reflection integral spectrum (UV-Vis DRIS), fluorescence spectra, TGA and single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group C2/c with a=31.110(8)A, b=11.544(3)A, c=22.583(6)A, β=112.419(3) o , V=7497(3)A 3 , Z=8, R 1 =0.0463 and wR 2 =0.1393 for unique 7686 reflections I>2σ(I). In the title compound, the Bi atoms have eight-fold and nine-fold coordination with respect to the oxygen atoms, with the Bi atoms in distorted dodecahedron and monocapped square antiprism, respectively. The 3-D framework of the title compound contains channels and is composed of linkages between Bi atoms and oxalate units, forming honeycomb-like layers with two kinds of 6+6 membered aperture, and pillared by oxalate ligands and monamide groups. The channels have N-ethylamine oxalate monamide group - CO 2 CONHCH 2 CH 2 NH 3 + , which is formed by the in situ reaction of en and oxalate acid. At room temperature, the complex exhibits intense blue luminescence with an emission peak at 445nm

1-(4-Methyl­phenyl­sulfon­yl)-5,6-di­nitro-1H-indazole

Science.gov (United States)

Oulemda, Bassou; Rakib, El Mostapha; Abbassi, Najat; Saadi, Mohamed; El Ammari, Lahcen

2014-01-01

In the title compound, C14H10N4O6S, the indazole ring system is almost perpendicular to the tosyl ring, as indicated by the dihedral angle of 89.40 (9)° between their planes. The dihedral angles between the indazole system and the nitro groups are 57.0 (3) and 31.9 (3)°. In the crystal, mol­ecules are linked by C—H⋯O inter­actions, forming chains running along [100]. PMID:24526962

2,5-Dimethyl-1-phenylsulfonyl-1H-pyrrole-3,4-dicarbaldehyde

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2009-03-01

Full Text Available In the title compound, C14H13NO4S, the mean planes of the pyrrole and phenyl rings form a dihedral angle of 88.7 (1°. The aldehyde groups are slightly twisted from the pyrrole plane. In the crystal structure, molecules are linked into a three-dimensional framework by C—H...O hydrogen bonds.

(1S,3S,4S-tert-Butyl N-[1-benzyl-3-hydroxy-5-phenyl-4-(picolinamidopentyl]carbamate

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Jian-Feng Zheng

2008-07-01

Full Text Available The title compound, C29H35N3O4, was obtained by the reaction of (2S,4S,5S-tert-butyl N-(4-amino-1-benzyl-3-hydroxy-5-phenylpentylcarbamate and picolinic acid using oxalyl chloride as a chlorinating reagent to activate the carboxyl group. In the crystal structure there are two molecules in the asymmetric unit, which are aligned edge-to-face. In one molecule, the pyridyl ring forms a dihedral angle of 22.0 (1° with the phenyl ring of the terminal benzyl group and 14.3 (1° with the other phenyl ring; in the other molecule, the corresponding angles are 12.1 (1 and 10.6 (1°, respectively. The packing is stabilized by intermolecular hydrogen bonds and C—H...π interactions.

1-[5-(Anthracen-9-yl-3-(4-nitrophenyl-4,5-dihydro-1H-pyrazol-1-yl]ethan-1-one

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Bao-Li Dong

2011-02-01

Full Text Available In the title compound, C25H19N3O3, steric repulsion between the methine H atom and one of the anthryl H atoms seems to be concomitant with the considerable distortion of the anthryl fragment from planarity. The side rings of the anthryl subtend an angle of 9.57 (8°, which is an extreme value among the known reliably determined structures. This angle correlates with the length of the bond by which the anthryl is attached to the rest of the molecule. In the anthryl fragment, the maximum deviation of one of the C atoms from the mean plane is 0.126 (3 Å and regards the carrier C atom involved in the repulsion between the anthryl and the methine H atoms. The interplanar angle between the pyrazoline ring and the anthryl fragment is 88.36 (5° and that between the pyrazoline and 4-nitrophenyl rings is 8.80 (15°. Weak intermolecular C—H...N, C—H...π and π–π interactions [centroid–centroid distances of 3.7659 (17, 3.9477 (15 and 3.8972 (15 Å] are pesent in the structure.

(3R,4Z-1,3-Diethyl-4-(2-oxopropylidene-2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one

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Laila El Foujji

2018-04-01

Full Text Available In the title compound, C16H20N2O2, the seven-membered ring adopts a bowl-shaped conformation while the orientation of the 2-oxopropylidene substituent is determined by an intramolecular N—H...O hydrogen bond, which generates an S(6 ring. In the crystal, inversion dimers linked by pairs of very weak C—H...O interactions occur, which generate R22(8 loops.

Bis(2-methyl-1H-imidazol-3-ium naphthalene-1,5-disulfonate dihydrate

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Yu-feng Wang

2012-06-01

Full Text Available The asymmetric unit of the title organic salt, 2C4H7N2+·C10H6O6S22−·2H2O, consists of a 2-methylimidazolium cation, a half of a naphthalene-1,5-disulfonate anion, which lies about a center of symmetry, and a water molecule. In the crystal, N—H...O and O—H...O hydrogen bonds link the cations, anions and water molecules into the layers parallel to (111.

2-(1H-Imidazol-1-yl)-3-isopropyl-1-benzothieno[3,2-d]pyrimidin-4(3H)-one

OpenAIRE

Xu, Sheng-Zhen

2007-01-01

In the title compound, C16H14N4OS, the three fused rings of the benzothieno[3,2-d]pyrimidinone unit are essentially coplanar, the maximum deviation from the mean plane being 0.067 (3) Å. The dihedral angle between the mean plane of the fused rings and the imidazole ring is 72.00 (3)°. Offset π–π stacking interactions involving the fused rings are effective in the stabilization of the crystal structure. The centroid–centroid distances between t...

{μ-2-[4-(1,3-Benzothiazol-2-ylphenyl]-2-azapropane-1,3-dithiolato-κ4S,S′:S,S′}bis[tricarbonyliron(I

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Da-yong Jiang

2012-03-01

Full Text Available The title compound, [Fe2(C15H12N2S3(CO6], was prepared as an azadithiolatodiiron model for the active site of [FeFe]-hydrogenase. The Fe2S2 core adopts a butterfly shape, with each metal having a pseudo square-pyramidal geometry. The N-substituted azadithiolate is μ2-κ4S,S′:S,S′-coordinated to the Fe(CO3 moieties to form two fused six-membered rings with different conformations. The sum of the C—N—C angles around the N atom [356.85 (15°] indicates a flattening of the trigonal–pyramidal geometry about the N atom and an increase in the degree of sp2-hybridization.

2,2-Dimethyl-2,3-dihydro-1H-perimidine

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Sarah Maloney

2013-02-01

Full Text Available The title compound, C13H14N2, was obtained from reaction of diaminonaphthalene with acetone. In both independent molecules in the asymmetric unit, the tricyclic perimidine consists of a planar (r.m.s. deviations = 0.0125 and 0.0181 Å naphthalene ring system and an envelope conformation C4N2 ringwith the NCN group hinged with respect to the naphthalene backbone by 36.9 (2 and 41.3 (2° in the two independent molecules. The methyl substituents are arranged approximately axial and equatorial on the apical C atom. In the crystal, one of the N—H groups of one independent molecule is involved in classical N—H...N hydrogen bonding. Short intermolecular (C/N—H...π(arene interactions, near the short T-shaped limit, link molecules in the absence of strong acceptors.

Synthesis of (+)-(3R)-3-(4-fluorophenylsulfonamido)-1,2,3,4-tetrahydro-9-[5,6,7,8,12,13-u-{sup 14}C]carbazoleppropanoic acid, [{sup 14}C]BAY u 3405

Energy Technology Data Exchange (ETDEWEB)

Radtke, M; Boberg, M; Pleiss, U [Inst. of Pharmacokinetics, Bayer AG, Wuppertal (Germany); Rosentreter, U [Pharma Production, Bayer AG. Wuppertal (Germany)

1994-12-01

The title compound [{sup 14}C]BAY u 3405 (1) was synthesized as part of 8-step sequence. Starting from [U-{sup 14}C]aniline hydrogensulfate the final product 1 was obtained with a specific activity of 741 MBq/mmol (20 mCi/mmol) and a radiochemical purity of > 98 % in an overall yield of 6 and 10 % depending on the method. (author).

[2,3,7,8,13,14,17,18-Octakis(ethylsulfanyl-5,10,15,20-porphyrazinato]zinc(II

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Mehmet Akkurt

2010-08-01

Full Text Available In the title compound, [Zn(C32H40N8S8], the ZnII ion is coordinated by four N atoms in a slightly distorted square-planar environment. In addition, there is a Zn...S contact involving a symmetry-related S atom which, when considered, forms a pseudo-square-pyramidal coordination with respect to the ZnII ion. Three of the ethyl groups are disordered over two sites with occupancy ratios of 0.841 (10:0.159 (10, 0.802 (10:0.198 (10 and 0.457 (13:0.543 (13. Weak intramolecular C—H...N and C—H...S interactions contribute to the stability of the molecular conformation. Intermolecular C—H...S contacts, weak C—H...π interactions and π–π stacking interactions [centroid–centriod distances = 3.832 (4 and 3.850 (5 Å] contribute to the stabilization of the crystal structure.

3-(1H-Indol-3-yl-2-(2-nitrobenzenesulfonamidopropanoic acid including an unknown solvate

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Islam Ullah Khan

2012-07-01

Full Text Available In the title compound, C17H15N3O6S, which crystallized with highly disordered methanol and/or water solvent molecules, the dihedral angle between the the indole and benzene ring systems is 5.3 (2°, which allows for the formation of intramolecular π–π stacking interactions [centroid–centroid separations = 3.641 (3 and 3.694 (3 Å] and an approximate overall U-shape for the molecule. In the crystal, dimers linked by pairs of Ns—H...Oc (s = sulfonamide and c = carboxylate hydrogen bonds generate R22(10 loops, whereas Ni—H...π (i = indole interactions lead to chains propagating in [100] or [010]. Together, these lead to a three-dimensional network in which the solvent voids are present as intersecting (two-dimensional systems of [100] and [010] channels. The title compound was found to contain a heavily disordered solvent molecule, which could be methanol or water or a mixture of the two. Due to its uncertain nature and the unresolvable disorder, the data were processed with the SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155], which revealed 877.8 Å3 of solvent-accessible volume per unit cell and 126 electron-units of scattering density or 109.7 Å3 (16 electron units per organic molecule.. This was not included in the calculations of overall formula weight, density and absorption coefficient.

(Z-3-(4-Chlorophenyl-1-(2,4-difluorophenyl-2-(1H-1,2,4-triazol-1-ylprop-2-en-1-one

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Xin-Mei Peng

2012-06-01

Full Text Available The asymmetric unit of the title compound, C17H10ClF2N3O, contains three independent molecules. In each molecule, the C=C bond has a cis conformation with respect to the triazole and chlorophenyl groups. The dihedral angles formed by the triazole ring with the diflurophenyl and chlorophenyl benzene rings, respectively, are 20.10 (14 and 73.22 (15, 25.31 (15 and 84.44 (15, and 16.44 (13 and 61.72 (14° in the three molecules while the dihedral angles between the benzene rings are 66.54 (13, 85.82 (12 and 58.37 (12°.

H1-A, a compound isolated from Fusarium oxysporum inhibits hepatitis C virus (HCV) NS3 serine protease.

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Yang, Li-Yuan; Lin, Jun; Zhou, Bin; Liu, Yan-Gang; Zhu, Bao-Quan

2016-04-01

The present study was aimed to isolate the active compounds from the fermentation products of Fusarium oxysporum, which had hepatitis C virus (HCV) NS3 protease inhibitory activity. A bioactive compound was isolated by reverse-phase silica-gel column chromatography, silica-gel column chromatography, semi-preparative reverse-phase High Performance Liquid Chromatography (HPLC), and then its molecular structure was elucidated based on the spectrosopic analysis. As a result, the compound (H1-A, 1) Ergosta-5, 8 (14), 22-trien-7-one, 3-hydroxy-,(3β, 22E) was isolated and identified. To the best of our knowledge, this was the first report on the isolation of H1-A from microorganisms with the inhibitory activity of NS3 protease. Copyright © 2016 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

Rethinking Sensitized Luminescence in Lanthanide Coordination Polymers and MOFs: Band Sensitization and Water Enhanced Eu Luminescence in [Ln(C15H9O5)3(H2O)3]n (Ln = Eu, Tb).

Science.gov (United States)

Einkauf, Jeffrey D; Kelley, Tanya T; Chan, Benny C; de Lill, Daniel T

2016-08-15

A coordination polymer [Ln(C15H9O9)3(H2O)3]n (1-Ln = Eu(III), Tb(III)) assembled from benzophenonedicarboxylate was synthesized and characterized. The organic component is shown to sensitize lanthanide-based emission in both compounds, with quantum yields of 36% (Eu) and 6% (Tb). Luminescence of lanthanide coordination polymers is currently described from a molecular approach. This methodology fails to explain the luminescence of this system. It was found that the band structure of the organic component rather than the molecular triplet state was able to explain the observed luminescence. Deuterated (Ln(C15H9O9)3(D2O)3) and dehydrated (Ln(C15H9O9)3) analogues were also studied. When bound H2O was replaced by D2O, lifetime and emission increased as expected. Upon dehydration, lifetimes increased again, but emission of 1-Eu unexpectedly decreased. This reduction is reasoned through an unprecedented enhancement effect of the compound's luminescence by the OH/OD oscillators in the organic-to-Eu(III) energy transfer process.

Synthesis, crystal structure and biological activity of a novel 1,2,3-thidiazole compound

International Nuclear Information System (INIS)

Ke, W.

2013-01-01

A new 1,2,3-thiadiazole compound was synthesized and characterized by 1H NMR, MS and HRMS. The crystal structure of the title compound (C/sub 12/H/sub 11/ClN/sub 2/O/sub 4/S/sub 2/, Mr = 346.80) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P-1 with a = 8.4425(17) A, b = 8.9801(18) A, c = 9.859(2) A, alpha = 84.36(3) degree, beta = 86.71(3)degree, lambda = 83.25(3) degree, V = 737.9(3)A3, Z 2, F(000) = 356, Dc = 1.561 g/cm/sup 3/, mu = 0.557 mm-1, the final R1 0.0380 and wR2 = 0.0982 for 2160 observed reflections with I > 2sigma(I). A total of 12585 reflections were collected, of which 2601 were independent (Rint 0.0364). The herbicidal activity of title compound was determined, the results showed the title compound displayed excellent herbicidal activity against Brassica campestris. (author)

A study of the reactions 14C( vector d, dprime)14C and 14C ( vector d, p)15C at 16.0 MeV

International Nuclear Information System (INIS)

Murillo, G.; Sen, S.; Darden, S.E.

1994-01-01

Cross-section and vector-analyzing-power measurements for 14 C(d, d prime) and 14 C(d, p) reactions have been carried out for E d =16 MeV. The inelastic-scattering data have been analyzed using the DWBA with a collective and a microscopic model form-factor and also by using the coupled-channels formalism with a vibrational model form-factor. It is observed that while the cross-section angular-distribution data for the two 2 + states at E x =7.012 and 8.318 MeV are very similar, the corresponding vector analyzing powers are quite different. The results of the analyses indicate that the distinctive characteristics probably arise from the difference in the relative importance of the proton and neutron components in the transition amplitude. The 3 - state at E x =6.728 MeV is identified as predominantly a 1p-3h state. Although the deformation parameters are relatively large, the single-particle structure aspects play a more dominant role than channel-coupling effects in populating the inelastic states. The transfer reaction data have been analyzed using the DWBA for bound and unbound states. The importance of two-step processes has been investigated via coupled-reaction-channels calculations. The g.s. and the states with excitation energies 0.770, 3.103 and 4.78 MeV in 15 C are populated primarily by a one-step process with a small two-step contribution in the case of the 3.103 MeV state. The 4.22 MeV state is populated predominantly by two-step processes. The 4.78 and the 5.83 MeV states have been identified as 1p-2h and 3p-4h, [3]/[2] + state, respectively, in an earlier report. There is close similarity in the level structures and reaction mechanisms between the states of 15 C and 17 O populated via the (d, p) reaction. ((orig.))

Preparation of 15N-13C-fulminic acid

International Nuclear Information System (INIS)

Wilmes, R.; Winnewisser, M.

1993-01-01

The precursor for the title compound was prepared in a three-step synthesis. The 13 C-label was incorporated in the first step employing 2- 13 C-ethyl acetate and the 15 N-label in the last step, using 15 N-sodium nitrite. Upon pyrolysis the precursor forms three fragments, one of them being the title compound. (Author)

3-Benzyl-4-ethyl-1H-1,2,4-triazole-5(4H-thione

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Zbigniew Karczmarzyk

2013-02-01

Full Text Available The title compound, C11H13N3S, exists in the 5-thioxo tautomeric form. The benzene ring exhibits disorder with a refined ratio of 0.77 (2:0.23 (2 for components A and B with a common bridgehead C atom. The 1,2,4-triazole ring is essentially planar, with a maximum deviation of 0.002 (3 Å for the benzyl-substituted C atom, and forms dihedral angles of 88.94 (18 and 86.56 (49° with the benzene rings of components A and B, respectively. The angle between the plane of the ethyl chain and the mean plane of 1,2,4-triazole ring is 88.55 (15° and this conformation is stabilized by an intramolecular C—H...S contact. In the crystal, pairs of N—H...S hydrogen bonds link molecules into inversion dimers. π–π interactions are observed between the triazole and benzene rings, with centroid–centroid separations of 3.547 (4 and 3.544 (12 Å for components A and B, and slippages of 0.49 (6 and 0.58 (15 Å, respectively.

(E-4-Hydroxy-6-methyl-3-[1-(2-phenylhydrazinylideneethyl]-2H-pyran-2-one

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Samra Rahmouni

2016-05-01

Full Text Available The title compound, C14H14N2O3, crystallized with three crystallographically independent molecules (A, B and C in the asymmetric unit. The three molecules each have an E conformation about the C=N bond but differ in the orientation of the phenyl and pyran rings. The dihedral angles between the phenyl and pyran ring planes are 14.30 (1, 28.38 (1 and 25.58 (1° in molecules A, B and C, respectively. There is an intramolecular O—H...N hydrogen bond in each molecule with an S(6 ring motif. In the crystal, molecules are linked by N—H...O and C—H...O hydrogen bonds, forming layers parallel to (001, enclosing R22(8 and R33(21 ring motifs. The layers are linked via C—H...π interactions, forming bilayers, which are joined by a further C—H...π interaction, forming a three-dimensional structure.

3-Methyl-1-(prop-2-en-1-ylquinoxalin-2(1H-one

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Youssef Ramli

2010-07-01

Full Text Available In the molecule of the title compound, C12H12N2O, the quinoxaline ring is planar with an r.m.s. deviation of 0.007 (15 Å. The dihedral angle between the quinoxaline and propenyl planes is 82.1 (2°. The crystal packing is stabilized by offset π–π stacking between the quinoxaline rings [centroid–centroid distance = 3.8832 (9 Å].

Synthesis of 15N-enriched urea (CO(15NH22 from 15NH3, CO, and S in a discontinuous process

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C. R. Sant Ana Filho

2012-12-01

Full Text Available CO(15NH22 enriched with the stable isotope 15N was synthesized based on a reaction involving CO, 15NH3, and S in the presence of CH3OH. The method differs from the industrial method; a stainless steel reactor internally lined with polytetrafluoroethylene (PTFE was used in a discontinuous process under low pressure and temperature. The yield of the synthesis was evaluated as a function of the parameters: the amount of reagents, reaction time, addition of H2S, liquid solution and reaction temperature. The results showed that under optimum conditions (1.36, 4.01, and 4.48 g of 15NH3, CO, and S, respectively, 40 ml CH3OH, 40 mg H2S, 100 ºC and 120 min of reaction 1.82 g (yield 76.5% of the compound was obtained per batch. The synthesized CO(15NH22 contained 46.2% N, 0.55% biuret, melting point of 132.55 ºC and did not exhibit isotopic fractionation. The production cost of CO(15NH22 with 90.0 at. % 15N was US$ 238.60 per gram.

(E)-6-Amino-1,3-dimethyl-5-[(pyridin-2-yl-methyl-idene)amino]-pyrimidine-2,4(1H,3H)-dione.

Science.gov (United States)

Booysen, Irvin; Hlela, Thulani; Ismail, Muhammed; Gerber, Thomas; Hosten, Eric; Betz, Richard

2011-09-01

In the title compound, C(12)H(13)N(5)O(2), a Schiff-base-derived chelate ligand, the non-aromatic heterocycle and its substituents essentially occupy one common plane (r.m.s. of fitted non-H atoms = 0.0503 Å). The N=C bond is E-configured. Intra-cyclic angles in the pyridine moiety cover the range 117.6 (2)-124.1 (2)°. Intra- and inter-molecular N-H⋯N and N-H⋯O hydrogen bonds are observed in the crystal structure, as are intra- and inter-molecular C-H⋯O contacts which, in total, connect the mol-ecules into a three-dimensional network. The shortest ring-centroid-to-ring-centroid distance of 3.5831 (14) Å is between the two different types of six-membered rings.

Ethyl 1-cyclopropyl-6,7-difluoro-8-methoxy-4-oxo-1,4-dihydroquinoline-3-carboxylate

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De-Cai Wang

2008-11-01

Full Text Available In the title compound, C16H15F2NO4, the dihedral angle between the three-membered ring and the quinoline ring system is 64.3 (3°. In the crystal structure, intermolecular C—H...O hydrogen bonds link the molecules, forming a column running along [101].

Ethyl (E-2-(2,7-dimethyl-5-oxo-4H,5H-pyrano[4,3-b]pyran-4-ylideneacetate

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Oulemda Bassou

2017-02-01

Full Text Available In the title compound, C14H14O5, the two heterocyclic rings are coplanar (r.m.s. deviation = 0.008 Å, with the largest deviation from the mean plane being 0.012 (1 Å. The mean plane through the acetate group is inclined slightly with respect to the oxopyrano[4,3-b]pyran-4-yl system, as indicated by the dihedral angle of 1.70 (7° between them. Two intramolecular hydrogen bonds, completing S(6 ring motifs, are observed in the molecule. In the crystal, molecules are linked by weak C—H...O hydrogen bonds involving the same acceptor atom, forming chains propagating along the c-axis direction and enclosing R21(6 ring motifs. The chains are linked via offset π–π interactions [intercentroid distance = 3.622 (1 Å], involving inversion-related oxopyrano[4,3-b]pyran-4-yl ring systems, forming slabs parallel to the bc plane.

Crystal structure of 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl) ethenyl]benzamide: N,N-dimethylformamide (1 : 1)

Energy Technology Data Exchange (ETDEWEB)

Sharma, P. [University of Jammu, X-ray Crystallography Laboratory, Department of Physics (India); Subbulakshmi, K. N.; Narayana, B. [Mangalore University, Department of Chemistry (India); Sarojini, B. K. [Mangalore University, Industrial Chemistry Division, Department of Studies in Chemistry (India); Kant, R., E-mail: rkant.ju@gmail.com [University of Jammu, X-ray Crystallography Laboratory, Department of Physics (India)

2016-03-15

The title compound, 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)ethenyl] benzamide:N,N-dimethylformamide (1: 1), (C{sub 15}H{sub 11}N{sub 3}O{sub 2}S{sub 2} · C{sub 3}H{sub 7}NO), was synthesized, and its structure was established by spectral analysis and X-ray diffraction studies. The compound crystallizes in the monoclinic space group P2{sub 1}/n with a = 10.8714(7), b = 9.0497(5), c = 19.8347(13) Å, β = 91.093(5)°, Z = 4. The crystal structure is stabilized by N–H···S, C–H···O and N–H···O hydrogen bonds. The π···π interactions are also observed between the rings.

2-(5-Fluoro-3-isopropylsulfanyl-1-benzofuran-2-ylacetic acid

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Pil Ja Seo

2011-11-01

Full Text Available The title compound, C13H13FO3S, was prepared by alkaline hydrolysis of ethyl 2-(5-fluoro-3-isopropylsulfanyl-1-benzofuran-2-ylacetate. In the crystal, the carboxy groups are involved in intermolecular O—H...O hydrogen bonds, which link the molecules into centrosymmetric dimers. These dimers are further packed into stacks along the b axis by a slipped π–π interaction between the furan and benzene rings of neighbouring molecules [centroid–centroid distance = 3.727 (2 Å, interplanar distance = 3.465 (2 Å and slippage = 1.373 (2 Å]. The crystal structure also exhibits a short S...O contact [S...O = 3.219 (2 Å].

Ring rearrangements and reactivity of 3-((4-oxo-4H-chromen-3-ylmethylene-4-phenyl-1H-[1,5]benzodiazepin-2(3H-one toward some nucleophiles

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Hanan Salah

2017-05-01

Full Text Available Condensation of 4-phenyl-1H-[1,5]benzodiazepin-2(3H-one (1 with 3-formylchromone (2 afforded a mixture of 3-(chromenylmethylene[1,5]benzodiazepinone 3 and 14-chromenylbenzodiazepino[2,3:6,5]pyrano[2,3-b]benzodiazepine 4. Ring rearrangements of compound 3 with different nucleophilic reagents, such as potassium hydroxide and/or ammonium acetate led to rearrangement into pyranobenzodiazepine 5 and pyridobenzodiazepine 6, respectively. Treatment of compound 3 with hydrazine hydrate, hydroxylamine hydrochloride, malononitrile, cyanothioacetamide, 2-cyano-3,3-disufanylacrylonitrile, and/or 2-cyano-3-phenylamino-3-sufanylacrylonitrile, has been carried out at different conditions, leading to versatile heterocyclic substituted benzodiazepines at position 3, viz. pyrazole 8, isoxazole 9, pyridines 10 and 11, 1,3-dithiine 12, and 1,3-thiazine 13 derivatives.

tert-Butyl 3-(8-bromo-4H,10H-1,2-oxazolo[4,3-c][1]benzoxepin-10-yl-2-methyl-1H-indole-1-carboxylate

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Ankur Trigunait

2010-08-01

Full Text Available In the title compound, C25H23BrN2O4, the seven-membered ring adopts a twisted-boat conformation. The indole ring system is planar within 0.021 (2 Å and the ester group [–C(=O—O—C–] is almost coplanar with it [dihedral angle = 3.0 (2°]. The conformation of the ester group is influenced by intramolecular C—H...O interactions. In the crystal structure, molecules are linked into chains along the b axis by C—H...N hydrogen bonds.

Butane-1,4-diyl bis(pyridine-4-carboxylate

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J. Muthukumaran

2011-07-01

Full Text Available The molecule of the title compound, C16H16N2O4, lies about an inversion centre; the butane chain adopts an extended zigzag conformation. The dihedral angle between the pyridine ring and the adjacent COO group is 3.52 (s14°.

2-(4-Bromophenyl-5-fluoro-3-phenylsulfinyl-1-benzofuran

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Hong Dae Choi

2010-08-01

Full Text Available In the title compound, C20H12BrFO2S, the O atom and the phenyl group of the phenylsulfinyl substituent lie on opposite sides of the plane through the benzofuran fragment; the phenyl ring is nearly perpendicular to this plane [dihedral angle = 86.98 (6°]. The 4-bromophenyl ring is rotated slightly out of the benzofuran plane, making a dihedral angle of 1.56 (8°. The crystal structure features aromatic π–π interactions between the furan and phenyl rings of neighbouring molecules [centroid–centroid distance = 3.506 (3 Å], and an intermolecular C—H...π interaction. The crystal structure also exhibits a short intermolecular S...S contact [3.2635 (8 Å].

Synthesis of binuclear rhodacarboranes from dianions 1,4- and 1,3-C6H4(CH2-9-C2H2B9H9-7,8-nido)22- and (Ph3P)3RhCl

International Nuclear Information System (INIS)

Zakharkin, L.I.; Zhigareva, G.G.

1996-01-01

Dianions 1,4 and 1,3-C 6 H 4 (CH 2 -9-C 2 H 2 B 9 H 9 -7,8-nido) 2 2- obtained from nido 7,8-dicarbollide-ion and 1,4-bis(bromomethyl) and 1,3-bis(bromomethyl)benzenes react with (Ph 3 P) 3 RhCl to give binuclear rhodacarboranes, 1,4- and 1,3-[3,3-(Ph 3 P) 2 -3-H-3,1,2-RhC 2 B 9 H 10 -4-CH 2 ] 2 C 6 H 6 with chemical reaction yield 85% and 87% respectively. 7 refs., 1 fig., 1 tab

Hydrates of the alkali trioxidomonosulfidomolybdates and -tungstates. K{sub 2}[(Mo/W)O{sub 3}S] . 1.5 H{sub 2}O and (Rb/Cs){sub 2}[(Mo/W)O{sub 3}S] . H{sub 2}O

Energy Technology Data Exchange (ETDEWEB)

Lehner, Anna J.; Braitsch, Milan; Roehr, Caroline [Freiburg Univ. (Germany). Inst. fuer Anorganische und Analytische Chemie

2012-11-01

The trioxidomonosulfidomolybdate and -tungstate anions [(Mo/W)O{sub 3}S]{sup 2-} are the first products formed when passing H{sub 2}S gas through a solution of the oxidometalates. Their potassium, rubidium and cesium salt hydrates form as crystalline precipitates from these solutions depending on pH, the polarity of the solvent, educt concentrations and temperature. The structures of the sesqui- (K) and mono- (Rb, Cs) hydrates have been determined by means of X-ray single crystal diffraction data. The potassium sesquihydrates K{sub 2}[(Mo/W)O{sub 3}S] . 1.5 H{sub 2}O are isotypic and crystallize with a new structure type (monoclinic, space group C2/c, M = Mo/W: a = 987.0(2)/993.13(11), b = 831.75(14)/831.10(11), c = 1868.9(4)/1865.2(2) pm, {beta} = 99.34(2)/99.153(8) , R1 = 0.0352/0.0390). In the crystal structure the [(Mo/W)O{sub 3}S]{sup 2-} anions are connected via hydrogen bonds to form columns along the c direction. Channels containing only water molecules run along the [101] direction. The dehydration process proceeds in a topotactic reaction between 60 to 95 C and yields crystals of the anhydrous salts K{sub 2}[(Mo/W)O{sub 3}S]. The two different K+ cations exhibit a 5 + 3 and 5 + 2 O/S coordination. The heavier alkali metal cations form the four monohydrates (Rb/Cs){sub 2}[(Mo/W)O{sub 3}S] . H{sub 2}O (trigonal rhombohedral, space group R anti 3m) with lattice parameters for the Rb/Cs molybdates of a = 621.17(6)/624.62(10), c = 3377.9(4)/3388.6(8) pm (R1 = 0.0505/0.0734) and the tungstates of a = 642.80(3)/643.3(4), c = 3532.8(3)/3566(4) pm (R1 = 0.0348/0.0660). In the structures the 3m symmetrical tetrahedra are arranged to form double layers in such a way, that the O{sub 3} bases of the tetrahedra are pointing towards each other in a staggered conformation. These double layers are stacked in the c direction in a rhombohedral sequence. In these hydrates, there are no distinct hydrogen bonds. Instead, partially disordered pairs of H{sub 2}O molecules are

1,3-Dibenzyl-6-bromo-1H-imidazo[4,5-b]pyridin-2(3H-one

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S. Dahmani

2010-04-01

Full Text Available The imidazopyridine fused-ring in the title compound, C20H16BrN3O, is planar (r.m.s. deviation = 0.011 Å. The phenyl rings of the benzyl substitutents twist away from the central five-membered ring in opposite directions; the rings are aligned at 61.3 (1 and 71.2 (1° with respect to this ring.

Crystal structure of 2-oxo-2H-chromen-7-yl 4-fluorobenzoate

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Akoun Abou

2018-05-01

Full Text Available In the title compound, C16H9FO4, (I, the benzene ring is oriented at an acute angle of 59.03 (15° relative to the coumarin plane (r.m.s deviation = 0.009 Å. This conformation of (I is stabilized by an intramolecular C—H...O hydrogen bond, which closes a five-membering ring. In the crystal, molecules of (I form infinite zigzag chains along the b-axis direction, linked by C—H...O hydrogen bonds. Furthermore, the crystal structure is supported by π–π stacking interactions between neighbouring pyrone and benzene or coumarin rings [centroid–centroid distances in the range 3.5758 (18–3.6115 (16 Å], as well as C=O...π interactions [O...centroid distances in the range 3.266 (3–3.567 (3 Å]. The theoretical data for (I obtained from quantum chemical calculations are in good agreement with the observed structure, although the calculated C—O—C—C torsion angle between the coumarin fragment and the benzene ring (73.7° is somewhat larger than the experimental value [63.4 (4°]. Hirshfeld surface analysis has been used to confirm and quantify the supramolecular interactions.

(2R,3aR,4S,7R,7aS,9R,10aR,11S,14R,14aS-rel-3a,4,7,7a,10a,11,14,14a-Octahydro-4,14:7,11-diepoxy-2,9-propanonaphtho[1,2-f:5,6-f′]diisoindole-1,3,8,10-tetrone (9CI: a cyclophane derived from naphtho[1,2-c:5,6-c]difuran

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Peter W. Dibble

2008-09-01

Full Text Available The title compound, C25H18N2O6, is a naphthalenophane styled in the manner of Warrener's alicyclic cyclophanes or molecular racks wherein a trimethylene tether is perfectly staggered between the two N atoms such that the central methylene H atoms point toward the naphthalene π-system. The dihedral angle between the mean planes of the two benzene rings is 7.61 (7°.

Ethyl 1-oxo-1,2,3,4-tetrahydro-9H-carbazole-3-carboxylate

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Tuncer Hökelek

2009-07-01

Full Text Available The title compound, C15H15NO3, contains a carbazole skeleton with an ethoxycarbonyl group at the 3 position. In the indole ring system, the benzene and pyrrole rings are nearly coplanar, forming a dihedral angle of 1.95 (8°. The cyclohexenone ring has an envelope conformation. In the crystal structure, pairs of strong N—H...O hydrogen bonds link the molecules into centrosymmetric dimers with R22(10 ring motifs. π–π contacts between parallel pyrrole rings [centroid–centroid distance = 3.776 (2 Å] may further stabilize the structure. A weak C—H...π interaction is also observed.

Three closely related (2E,2′E-3,3′-(1,4-phenylenebis[1-(methoxyphenylprop-2-en-1-ones]: supramolecular assemblies in one dimension mediated by hydrogen bonding and C—H...π interactions

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Aijia Sim

2017-06-01

Full Text Available In the title compounds, (2E,2′E-3,3′-(1,4-phenylenebis[1-(2-methoxyphenylprop-2-en-1-one], C26H22O4 (I, (2E,2′E-3,3′-(1,4-phenylenebis[1-(3-methoxyphenylprop-2-en-1-one], C26H22O4 (II and (2E,2′E-3,3′-(1,4-phenylenebis[1-(3,4-dimethoxyphenylprop-2-en-1-one], C28H26O6 (III, the asymmetric unit consists of a half-molecule, completed by crystallographic inversion symmetry. The dihedral angles between the central and terminal benzene rings are 56.98 (8, 7.74 (7 and 7.73 (7° for (I, (II and (III, respectively. In the crystal of (I, molecules are linked by pairs of C—H...π interactions into chains running parallel to [101]. The packing for (II and (III, features inversion dimers linked by pairs of C—H...O hydrogen bonds, forming R22(16 and R22(14 ring motifs, respectively, as parts of [201] and [101] chains, respectively.

(E-3-Methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone

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Yordanka Ivanova

2016-04-01

Full Text Available The title compound, (E-3-methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone, was synthesized by Claisen-Schmidt condensation of 3-methyl-2(3H-benzothiazolone-6-carbaldehyde with 2-acetylthiophene in 94% yield. The structure of the target compound was confirmed using 1H-NMR, 13C-NMR, IR, MS, and elemental analysis.

A novel synthesis of octahydropyrido[3,2-c]carbazole framework of aspidospermidine alkaloids and a combined computational, FT-IR, NMR, NBO, NLO, FMO, MEP study of the cis-4a-Ethyl-1-(2hydroxyethyl)-2,3,4,4a,5,6,7,11c-octahydro-1H-pyrido[3,2-c]carbazole

Science.gov (United States)

Uludağ, Nesimi; Serdaroğlu, Goncagul; Yinanc, Abdullah

2018-06-01

In this study, we performed a novel synthesis of the octahydropyrido[3,2-c]carbazole derivative 6 from 1 in five steps with a 34% overall yield. We also developed a unique compound 2 by a cyclization reaction from the cyanoethylation of compound 1, which is an intermediate step in the synthesis of Aspidospermidine. The parent compound of Aspidospermidine alkaloids, comprise a large family of diverse structures. As a result, we obtained octahydropyrido[3,2-c]carbazole (6)and the proposed method may be applicable to other alkaloids. All quantum chemical calculations of the cis-4a-Ethyl-1-(2-hydroxyethyl)-2,3,4,4a,5,6,7,11c-octahydro-1H-pyrido[3,2-c]carbazole have been performed with the DFT/B3LYP and HF methods by using the Gaussian 09W software package. The most stable conformer obtained from the Potential Energy Surface (PES) scan analysis at the B3LYP/6-31G** level of theory in the gas phase was used as the starting structure of the title compound to further computational analysis. The Natural Bond Orbital (NBO) and NLO analyses were performed to evaluate the intra-molecular interactions contributing to the molecular stability and to predict the optical properties of the title compound, respectively. Gauge-Independent Atomic Orbital (GIAO) approach was used to determine the 1H and 1C NMR chemical shifts of the title compound by subtracting the shielding constants of TMS at both methods. The calculated vibrational frequencies of the title compound were assigned by using the VEDA program and were scaled down by using the scaling factor 0.9668 for B3LYP/6-311++G(d, p) and 0.9050 for HF/6-311++G(d, p) to improve the calculated vibrational frequencies. The FMO (frontier molecular orbital) analysis was evaluated to predict the chemical and physical properties of the title compound and the HOMO, LUMO, and MEP diagrams were visualized by GaussView 4.1 program to present the reactive site of the title compound.

catena-Poly[[[trans-diaquabis(pyridine-κNcobalt(II]-μ-(4-{N′-[1-(3-acetyl-4-methyl-1H-pyrazol-5-ylethylidene]hydrazino}benzoato-κ3O:N,N′-[bis(pyridine-κNcobalt(III]-μ-(4-{N′-[1-(3-acetyl-4-methyl-1H-pyrazol-5-ylethylidene]hydrazino}benzoato-κ3N,N′:O]perchlorate 3.66-hydrate

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Igor O. Fritsky

2008-02-01

Full Text Available The title compound, {[Co2(C15H14N4O32(C5H5N4(H2O2]ClO4·3.66H2O}n, is a one-dimensional coordination polymer, with both CoII and CoIII centres in its structure. The ligand environment surrounding CoIII is formed by two N,N-chelating pyrazole-containing ligands and two pyridine molecules in axial positions. The high-spin CoII ions, situated at crystallographic centres of inversion, exhibit a distorted octahedral coordination mode. The ClO4− anion is linked to the polymer chain via hydrogen bonds. The chains are connected by hydrogen bonds to produce a three-dimensional structure.

2,2-Dimethyl-2,3-dihydropyrano[2,3-a]carbazol-4(11H-one

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Makuteswaran Sridharan

2008-11-01

Full Text Available The title compound, C17H15NO2, was prepared from 1-hydroxycarbazole and 3,3-dimethylacrylic acid with a mixture of AlCl3 and POCl3 as the cyclization catalyst. Owing to the presence of the –CMe2– group, the molecule is not quite planar. In the crystal structre, strong N—H...O hydrogen bonds and weaker C—H...π interactions occur, and a slipped π–π stacking interaction [centroid–centroid separation = 3.8425 (8 Å] is also observed.

Tris(dibenzoylmethanido-κ2O,O′[(6S,8S-(+-7,7-dimethyl-3-(2-pyridyl-5,6,7,8-tetrahydro-6,8-methanoisoquinoline-κ2N,N′]gadolinium(III

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Xi-Li Li

2009-09-01

Full Text Available In the title compound, [Gd(C15H11O23(C17H18N2], the GdIII atom is coordinated by six O atoms from three β-diketonate ligands and two N atoms from a chiral ligand LS,S-(+-7,7-dimethyl-3-(2-pyridyl-5,6,7,8-tetrahydro-6,8-methanoisoquinoline, in a coordination geometry best described as distorted square-antiprismatic.

2,5,11,14-Tetraoxa-8-azadispiro[13.4.0]nonadeca-15,17,19-triene

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Quanying Gan

2010-05-01

Full Text Available The title compound, C14H21NO4, has been synthesized from o-dihydroxybenzene by a three-step reaction. There are two chemically equal but crystallographically independent molecules in the asymmetric unit. The crystal packing is governed by C—H...O hydrogen bonds and C—H...π interactions, forming an infinite network.

7-Fluoro-4-oxochromene-3-carbaldehyde

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Mohammad Asad

2011-04-01

Full Text Available In the title compound, C10H5FO3, the chromenone ring is essentially planar, with a maximum deviation of 0.039 (1 Å. The dihedral angle between the fluoro-subsituted benzene ring and the pyran ring is 1.92 (4°. In the crystal, molecules are connected via weak intermolecular C—H...O hydrogen bonds, forming supramolecular ribbons along the b axis. These ribbons are stacked down the a axis.

Synthesis of a cleavable heterobifunctional photolabelling reagent: ring-labelled 3-((4-azidophenyl)dithio)propionic acid- sup 14 C

Energy Technology Data Exchange (ETDEWEB)

Ramaswami, Varadarajan (Carnegie-Mellon Univ., Pittsburgh, PA (USA). Dept. of Chemistry); Tirrell, D.A. (Massachusetts Univ., Amherst, MA (USA). Dept. of Polymer Science and Engineering)

1989-08-01

An efficient synthesis of ring-labelled 3-((4-azidophenyl)dithio)propionic acid-{sup 14}C is described. Chlorosulfonation of uniformly ring-labelled acetanilide-{sup 14}C followed by reductive dimerization of the sulfonyl chloride with HI afforded 4-acetamidophenyl disulfide. Hydrolysis and diazotization then gave 4-azidophenyl disulfide, which was converted to the title compound via the sulfur transfer reagent N-(4-azidophenylthio)phthalimide. The overall yield of 3-((4-azidophenyl)dithio)propionic acid-{sup 14}C was 22%. 3-((4-Azidophenyl)dithio)propionic acid-{sup 14}C is a cleavable heterobifunctional photolabelling reagent of potential utility in studies of biomembrane structure and intermacromolecular interaction. (author).

(4S)-4-(3,4-Dichloro?phen?yl)-1?-methyl-4?-phenyl-3,4-dihydronaphthalene-2-spiro-3?-pyrrolidine-2?-spiro-1??-acenaphthyl?ene-1,2??(2H,1??H)-dione

OpenAIRE

Murugan, R.; Gunasekaran, B.; Narayanan, S. Sriman; Manivannan, V.

2008-01-01

In the title compound, C37H27Cl2NO2, the 3,4-dichloro?phenyl ring makes a dihedral angle of 46.66?(6)? with the phenyl ring. The mol?ecular structure is stabilized by weak intra?molecular C?H?O inter?actions and the crystal structure is stabilized by weak inter?molecular C?H?O inter?actions. The C?C?C?C?C five-membered ring is planar, while the C?C?C?C?N five-membered ring adopts a half-chair conformation.

Crystal structure of 1-(2,4-dimethylphenyl-2-(4-trimethylsilyl-1H-1,2,3-triazol-1-ylethanone

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G. B. Venkatesh

2014-12-01

Full Text Available The asymmetric unit of the title compound, C15H21N3OSi, contains two molecules with similar conformations (r.m.s. overlay fit for the 20 non-H atoms = 0.163 Å. The dihedral angles between the planes of the 1,2,3-triazole and 2,4-dimethylbenzene rings are 27.0 (3 and 19.5 (3°. In the crystal, molecules are linked by very weak C—H...O and C—H...N hydrogen bonds to generate [100] chains. The chains are cross-linked by C—H...π interactions.

(μ-2,3-Dihydroxybutane-1,4-dithiolatobis[triphenyltin(IV

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Cuiping Li

2010-02-01

Full Text Available In the title compound, [Sn2(C6H56(C4H8O2S2], the geometry around the Sn atoms is distorted tetrahedral. The hydroxy groups are involved in O—H...O hydrogen bonding, which connects molecules into centrosymmetric dimers.

The crystal structure of Cs{sub 2}S{sub 2}O{sub 3}.H{sub 2}O

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Winkler, Verena; Schlosser, Marc; Pfitzner, Arno [Regensburg Univ. (Germany). Inst. fuer Anorganische Chemie

2016-08-01

A reinvestigation of the alkali metal thiosulfates has led to the new phase Cs{sub 2}S{sub 2}O{sub 3}.H{sub 2}O. At first cesium thiosulfate monohydrate was obtained as a byproduct of the synthesis of Cs{sub 4}In{sub 2}S{sub 5}. Further investigations were carried out using the traditional synthesis reported by J. Meyer and H. Eggeling. Cs{sub 2}S{sub 2}O{sub 3}.H{sub 2}O crystallizes in transparent, colorless needles. The crystal structure of the title compound was determined by single crystal X-ray diffraction at room temperature: space group C2/m (No. 12), unit cell dimensions: a = 11.229(4), b = 5.851(2), c = 11.260(5) Aa, β = 95.89(2) , with Z = 4 and a cell volume of V = 735.9(5) Aa{sup 3}. The positions of all atoms including the hydrogen atoms were located in the structure refinement. Cs{sub 2}S{sub 2}O{sub 3}.H{sub 2}O is isotypic with Rb{sub 2}S{sub 2}O{sub 3}.H{sub 2}O. Isolated tetrahedra [S{sub 2}O{sub 3}]{sup 2-} are coordinated by the alkali metal cations, and in addition they serve as acceptors for hydrogen bonding. For both Cs atoms the shortest distances are observed to oxygen atoms of the S{sub 2}O{sub 3}{sup 2-} anions whereas the terminating sulfur atom has its shortest contacts to the water hydrogen atoms. Thus, an extended hydrogen bonding network is formed. The title compound has also been characterized by IR spectroscopy. IR spectroscopy reveals the vibrational bands of the water molecules at 3385 cm{sup -1}. They show a red shift in the OH stretching and bending modes as compared to free water. This is due both to the S..H hydrogen bonding and to the coordination of H{sub 2}O molecules to the cesium atoms.

Neutron diffraction analysis of HRh[P(C6H5)3]4

International Nuclear Information System (INIS)

Bau, R.; Stevens, R.C.; McLean, M.; Koetzle, T.F.

1987-01-01

We have collected neutron diffraction data on a large single crystal of the title compound. The most surprising result is an extremely short Rh-H distance of 1.31(8) A, presumably caused by steric interactions involving the bulky triphenyl phosphine ligands. Crystallographic details: HRh[P(C 6 H 5 ) 3 ] 4 . 1 / 2 C 6 H 6 crystallizes in the space group Pa3, with a = b = c = 22.776(3) A, Z = 8. Data were collected at the Brookhaven High Flux Beam reactor at a temperature of -23 0 C, λ = 1.15882(7) A -1 . Least-squares refinement (in which the phenyl rings were treated as rigid groups) resulted in an R factor [based on data with f > 4σ(F)] of 0.12 for 914 reflections and 95 parameters. 10 refs

3-Benzyl-4-ethyl-1H-1,2,4-triazole-5(4H)-thione.

Science.gov (United States)

Karczmarzyk, Zbigniew; Pitucha, Monika; Wysocki, Waldemar; Pachuta-Stec, Anna; Stańczuk, Andrzej

2013-02-01

The title compound, C(11)H(13)N(3)S, exists in the 5-thioxo tautomeric form. The benzene ring exhibits disorder with a refined ratio of 0.77 (2):0.23 (2) for components A and B with a common bridgehead C atom. The 1,2,4-triazole ring is essentially planar, with a maximum deviation of 0.002 (3) Å for the benzyl-substituted C atom, and forms dihedral angles of 88.94 (18) and 86.56 (49)° with the benzene rings of components A and B, respectively. The angle between the plane of the ethyl chain and the mean plane of 1,2,4-triazole ring is 88.55 (15)° and this conformation is stabilized by an intra-molecular C-H⋯S contact. In the crystal, pairs of N-H⋯S hydrogen bonds link mol-ecules into inversion dimers. π-π inter-actions are observed between the triazole and benzene rings, with centroid-centroid separations of 3.547 (4) and 3.544 (12) Å for components A and B, and slippages of 0.49 (6) and 0.58 (15) Å, respectively.

15C-15F Charge Symmetry and the 14C(n,γ)15C Reaction Puzzle

International Nuclear Information System (INIS)

Timofeyuk, N.K.; Thompson, I.J.; Baye, D.; Descouvemont, P.; Kamouni, R.

2006-01-01

The low-energy reaction 14 C(n,γ) 15 C provides a rare opportunity to test indirect methods for the determination of neutron capture cross sections by radioactive isotopes versus direct measurements. It is also important for various astrophysical scenarios. Currently, puzzling disagreements exist between the 14 C(n,γ) 15 C cross sections measured directly, determined indirectly, and calculated theoretically. To solve this puzzle, we offer a strong test based on a novel idea that the amplitudes for the virtual 15 C→ 14 C+n and the real 15 F→ 14 O+p decays are related. Our study of this relation, performed in a microscopic model, shows that existing direct and some indirect measurements strongly contradict charge symmetry in the 15 C and 15 F mirror pair. This brings into question the experimental determinations of the astrophysically important (n,γ) cross sections for short-lived radioactive targets

5-tert-Butyl 3-ethyl 1-isopropyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine-3,5-dicarboxylate

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Huan-Mei Guo

2011-12-01

Full Text Available In the title compound, C17H27N3O4, the six-membered ring adopts a half-chair conformation with the N atom and the adjacent methylene C atom displaced by −0.391 (2 and 0.358 (2 Å, respectively, from the plane of the other four atoms. In the crystal, molecules are linked by weak C—H...O interactions.

New homo- and heteroleptic derivatives of trivalent ytterbium containing anion-radical 1,4-diazadiene ligands. Synthesis, properties and crystal structure of (C9H7)2Yb[2-MeC6H4NC(Me)C(Me)NC6H4Me-2] and [PhNC(Ph)C(Ph)NPh]3Yb complexes

International Nuclear Information System (INIS)

Gudilenkov, I.D.; Fukin, G.K.; Cherkasov, A.V.; Shavyrin, A.S.; Trifonov, A.A.; Larionova, Yu.E.

2008-01-01

Reaction of ytterbium bisindenyl complex (C 9 H 7 ) 2 Yb II (THF) 2 (1) with 1,4-diazabutadiene 2-MeC 6 H 4 N=C(Me)-C(Me)=NC 6 H 4 Me-2 ( Me DAD) is accompanied by the oxidation of metal atom until trivalent state and results in the formation of paramagnetic compound of metallocenes type (C 9 H 7 ) 2 Yb III ( Me DAD -. ) (3) containing 1,4-diazabutadiene anion-radical. Structure of complex 3 is ascertained by the X-ray structure analysis. Reactions of bisindenyl (1) and bisfluorenyl (C 13 H 9 ) 2 Yb II (THF) 2 (2) derivatives of bivalent ytterbium with 1,4-diazabutadiene PhN=C(Ph)-C(Ph)=NPh ( Ph DAD) (at 1:2 molar ratio of reagents) proceed with the complete break of Yb-C bonds, oxidation of ytterbium atom until trivalent state, and result in the formation of homoligand complex ( Ph DAD -. ) 3 Yb (6) containing three anion-radical 1,4-diazadiene ligands. Complex 6 was also prepared by the exchange reaction of YbCl 3 with Ph DAD -. K + (1:3) in THF. Complex 6 is characterized by the X-ray structure analysis [ru

4-Hydroxy-6-methyl-3-[3-(thiophen-2-ylacryloyl]-2H-pyran-2-one

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Salima Thabti

2013-04-01

Full Text Available The title compound, C13H10O4S, crystallizes with two molecules in the asymmetric unit in which the rings make dihedral angles of 3.9 (1 and 6.0 (1°; this planarity is due in part to the presence of an intramolecular O—H...O hydrogen bond, which generates an S(6 ring in each molecule. Both molecules represent E isomers with respect to the central C=C bond. In the crystal, molecules are linked by C—H...O interactions into a three-dimensional network.

The Determination of Sub-Microgram Quantities, of Amino Acids with H{sup 3}- and C{sup 1}4-Labelled 1-Fluoro-2.4 Dinitrobenzene; Determination d'acides amines en quantites inferieures au microgramme a l'aide de 1-fluoro-2,4-dinitrobenzen e marque au {sup 3}H et au {sup 14}C; Podschet submikrogrammnykh kolichestv aminokislot pri pomoshchi 2 : 4 dinitroftor'enzola, mechennogo H{sup 3} i C{sup 14}; Determinacion de cantidades de aminoacidos inferiores al microgramo por medio de 1-fluoro-2,4-dinitrobenceno marcado con {sup 3}H y {sup 14}C

Energy Technology Data Exchange (ETDEWEB)

Beale, D; Whitehead, J K [Middlesex Hospital Medical School, London (United Kingdom)

1962-01-15

satisfactoriament con los valores que suministra el analisis por derivacion empleando anhidrido acetico marcado con {sup 3}H y con {sup 14}C, y con los que se obtienen mediante cromatografia de intercambio ionico. (author) [Russian] Opisyvaetsya metod izotopnogo derivatsionnogo analiza dlya opredeleniya aminokislot pri nizkom urovne v 10{sup -5} mikro-mol' v gidrolizatakh proteina. 2:4 djnitroftorbenzola-H{sup 3} (G) byl sintezirovan iz ' brombenzola-H{sup 3}(G) i 2 : 4 dinitroftorbenzola-C{sup 14}(G), kotoryj byl poluchen iz khlorbenzola-C{sup 14}(G). Metod analiza vklyuchaet obrabotku smesi amino-kislot tritirovannym reaktivom (udel'naya aktivnost' 12.8 mikro kyuri/mikro ehkvijalent) v shchelochnoj rastvore, k kotoromu prisoedinyaetsya primes' s izvestnoj aktivnost' (6000 raspadov v minutu) proizvodnykh 2 : 4 dinitrofenila , mechennogo S14. Posle rastvoryayushchej ehkstraktsii smeshannaya reaktsiya vydelyaet iz svoego sostava proizvodnye dinitrofinila dvumya putyami khromatografii na bumage i soderzhanie H''3 i C''1''4 kazhdoj kapli opredelyaetsya szhiganiem i gazovym podschetom. Podschet H''3 daet kolichestvo, ravnoe proizvodnoj DNK iz aminokisloty, otdelennoj ot osnovnoj smesi, a schet C''1''4 ukazyvaet na velichinu poter', poluchivshikhsya vo vremya analiza. Itogi, poluchennye v rezul'tate analiza 1 mikrogramma gidrolizovannogo insulina polnost'yu soglasuyutsya s velichinami, poluchennymi v rezul'tate derivatsionnogo analiza s ispol'zovaniem uksusnogo angidrida, mechennogo H{sup 3} i C{sup 14} i s pomoshch'yu khromotografii ionnogo obmena smol. (author)

Multiple C-H Bond Activations and Ring-Opening C-S Bond Cleavage of Thiophene by Dirhenium Carbonyl Complexes.

Science.gov (United States)

Adams, Richard D; Dhull, Poonam; Tedder, Jonathan D

2018-06-14

The reaction of Re 2 (CO) 8 (μ-C 6 H 5 )(μ-H) (1) with thiophene in CH 2 Cl 2 at 40 °C yielded the new compound Re 2 (CO) 8 (μ-η 2 -SC 4 H 3 )(μ-H) (2), which contains a bridging σ-π-coordinated thienyl ligand formed by the activation of the C-H bond at the 2 position of the thiophene. Compound 2 exhibits dynamical activity on the NMR time scale involving rearrangements of the bridging thienyl ligand. The reaction of compound 2 with a second 1 equiv of 1 at 45 °C yielded the doubly metalated product [Re 2 (CO) 8 (μ-H)] 2 (μ-η 2 -2,3-μ-η 2 -4,5-C 4 H 2 S) (3), formed by the activation of the C-H bond at the 5 position of the thienyl ligand in 2. Heating 3 in a hexane solvent to reflux transformed it into the ring-opened compound Re(CO) 4 [μ-η 5 -η 2 -SCC(H)C(H)C(H)][Re(CO) 3 ][Re 2 (CO) 8 (μ-H)] (4) by the loss of one CO ligand. Compound 4 contains a doubly metalated 1-thiapentadienyl ligand formed by the cleavage of one of the C-S bonds. When heated to reflux (125 °C) in an octane solvent in the presence of H 2 O, the new compound Re(CO) 4 [η 5 -μ-η 2 -SC(H)C(H)C(H)C(H)]Re(CO) 3 (5) was obtained by cleavage of the Re 2 (CO) 8 (μ-H) group from 4 with formation of the known coproduct [Re(CO) 3 (μ 3 -OH)] 4 . All new products were characterized by single-crystal X-ray diffraction analyses.

(E-4-Bromo-N-(2,3-dimethoxybenzylideneaniline

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Karla Fejfarová

2010-09-01

Full Text Available The title Schiff base compound, C15H14BrNO2, was prepared by the condensation of 2,3-dimethoxybenzaldehyde with 4-bromoaniline. It adopts an E configuration with respect to the C=N bond. The dihedral angle between the two aromatic rings is 56.79 (8°. Weak C—H...O and C—-H...π bonds can be found in the crystal structure.

{2-[Bis(2,4-di-tert-butylphenoxyphosphanyloxy-κP]-3,5-di-tert-butylphenyl-κC1}[(1,2,5,6-η-cycloocta-1,5-diene]rhodium(I toluene monosolvate

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Detlef Selent

2012-02-01

Full Text Available The reaction of (η3-allyl[(1,2,5,6-η-cycloocta-1,5-diene]rhodium(I with tris(2,4-di-tert-butylphenylphosphite in toluene produces the title compound, [Rh(C42H62O3P(C8H12]·C7H8, by spontaneous metallation at one of the nonsubstituted phenyl ortho-C atoms of the phosphite molecule. The coordination geometry at the RhI ion is distorted square-planar. The toluene solvent molecule is disordered over two different orientations, with site-occupation factors of 0.810 (2 and 0.190 (2.

Crystal structure of a diaryl carbonate: 1,3-phenylene bis(phenyl carbonate

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Marina A. Solomos

2017-12-01

Full Text Available The whole molecule of the title compound, C20H14O6, is generated by mirror symmetry, the mirror bisecting the central benzene ring. The carbonate groups adopt an s-cis-s-cis conformation, with torsion angles of 58.7 (2 and 116.32 (15°. The crystal structure of 1,3-phenylene bis(phenyl carbonate contains no strong hydrogen bonds, though weak C—H...O and offset π–π interactions are observed, forming layers parallel to the ac plane.

catena-Poly[[[diaqua(2-fluorobenzoato-κ2O,O′strontium]-μ3-2-fluorobenzoato-κ5O:O,O′:O′,F] monohydrate

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Zhu-Nian Jin

2011-04-01

Full Text Available In the title compound, {[Sr(C7H4FO22(H2O2]·H2O}n, the SrII atom is coordinated by six O atoms and one F atom from four 2-fluorobenzoate ligands and two water molecules, resulting in an irregular SrFO8 coordination environment. The μ3-2-fluorobenzoate ligand bridges three symmetry-related SrII atoms, giving rise to a chain structure extending along [010]. The polymeric chains are connected via O—H...O hydrogen bonds into a two-dimensional supramolecular structure parallel to (100.

Et2NH2C6H3(CO23SnBr2.4H2O: SYNTHESIS AND INFRARED STUDY

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DAOUDA NDOYE

2014-01-01

Full Text Available The title compound has been obtained on allowing [C6H3(CO23(Et2NH23] to react with SnBr4. The molecular structure of Et2NH2C6H3(CO23SnBr2.4H2O has been determined on the basis of the infrared data. The suggested structure is a dimer in which each tin atom is hexacoordinated by two chelating C6H3(CO233- anions and two Br atoms. Cy2NH2+cations are involved through hydrogen bonds with non-coordinating CO2 groups. The suggested structure is a cage.

(E-3-Propoxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one monohydrate

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Burkhon Zh Elmuradov

2010-05-01

Full Text Available The title compound, C15H16N2O2·H2O, was synthesized via the alkylation of 3-hydroxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one with n-propyl iodide in the presence of sodium hydroxide. The organic molecule and the water molecule both lie on a crystallographic mirror plane. In the crystal structure, intermolecular O—H...O and O—H...N hydrogen bonds link the components into extended chains along [100].

3-{2-[2-(2-Fluorobenzylidenehydrazinyl]-1,3-thiazol-4-yl}-2H-chromen-2-one

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Afsheen Arshad

2010-06-01

Full Text Available In the title compound, C19H12FN3O2S, the chromene ring system and the thiazole ring are approximately planar [maximum deviations of 0.023 (3 Å and 0.004 (2 Å, respectively]. The chromene ring system is inclined at angles of 4.78 (10 and 26.51 (10° with respect to the thiazole and benzene rings, respectively, while the thiazole ring makes a dihedral angle of 23.07 (12° with the benzene ring. The molecular structure is stabilized by an intramolecular C—H...O hydrogen bond, which generates an S(6 ring motif. The crystal packing is consolidated by intermolecular N—H...O hydrogen bonds, which link the molecules into chains parallel to [100], and by C—H...π and π–π [centroid–centroid distance = 3.4954 (15 Å] stacking interactions.

Isotope effects and their implications for the covalent binding of inhaled [3H]- and [14C]formaldehyde in the rat nasal mucosa

International Nuclear Information System (INIS)

Heck Hd'; Casanova, M.

1987-01-01

DNA-protein crosslinks were formed in the nasal respiratory mucosa of Fischer-344 rats exposed for 3 hr to selected concentrations of [ 3 H]- and [ 14 C]formaldehyde ( 3 HCHO and H 14 CHO). In rats depleted of glutathione (GSH) and exposed to 10 ppm of 3 HCHO and H 14 CHO, the 3 H/ 14 C ratio of the fraction of the DNA that was crosslinked to proteins was significantly (39 +/- 6%) higher than that of the inhaled gas. This suggests an isotope effect, either on the formation of DNA-protein crosslinks by labeled HCHO or on the oxidation of labeled HCHO catalyzed by formaldehyde (FDH) or aldehyde dehydrogenase (AldDH). The possibility of an isotope effect on the formation of crosslinks was investigated using rat hepatic nuclei incubated with [ 3 H]- and [ 14 C]formaldehyde (0.1 mM, 37 degrees C). A small (3.4 +/- 0.9%) isotope effect was detected on this reaction, which slightly favored 3 HCHO over H 14 CHO in binding to DNA. The magnitude of this isotope effect cannot account for the high isotope ratio observed in the crosslinked DNA in vivo. The possibility of an isotope effect on the oxidation of 3 HCHO and H 14 CHO catalyzed by FDH was investigated using homogenates of the rat nasal mucosa incubated with [ 3 H]- and [ 14 C]formaldehyde at total formaldehyde concentrations ranging from 0.1 to 11 microM, NAD+ (1 mM), GSH (15 mM), and pyrazole (1 mM). The experiments showed that 3 HCHO is oxidized significantly more slowly than H 14 CHO under these conditions (Vmax/Km (H 14 CHO) divided by Vmax/Km ( 3 HCHO) = 1.82 +/- 0.11). A similar isotope effect was observed in the absence of GSH, presumably due to the oxidation of 3 HCHO and H 14 CHO catalyzed by AldDH

DFT calculations on 1,4-dithiine and S-oxygenated derivatives

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E. Vessally

2008-12-01

Full Text Available The molecular structures of 1,4-dithiine and S-oxygenated derivatives are studied using B3LYP/6-311++G** level of theory. These compounds have 8π-electrons in the ring. This led to stabilization of non-planar conformation. DFT calculations show that 1,4-dithiine, C4H4SS, 1,4-dithiine-1-oxide, C4H4SOS, 1,4-dithiine-1,4-dioxide, C4H4SOSO and 1,4-dithiine-1,1,4-trioxide, C4H4SO2SO; have boat conformation. 1,4-dithiine-1,1-dioxide, C4H4SO2S, have a shadow boat conformation. 1,4-dithiine-1,1,4,4-tetraoxide, C4H4SO2SO2, have a planar conformation.

5-[(3,5-Dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-1,3-diethyl-2-thioxodihydropyrimidine-4,6(1H,5H-dione

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Salman A. Khan

2010-03-01

Full Text Available The title compound, 5-[(3,5-dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-1,3-diethyl-2-thioxodihydropyrimidine-4,6(1H,5H-dione, has been synthesized by condensation of 1,3-diethyl-2-thiobarbituric acid and 3,5-dimethyl-1-phenylpyrazole-4-carbaldehyde in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H-NMR, 13C-NMR and EI-MS spectral analysis.

Synthesis, crystal structure, spectral analysis, dft studies and antimicrobial activity of ethyl 6-(4-(ethoxycarbonyl)-1h-1,2,3-triazol-1-yl)pyridine-3-carboxylate

International Nuclear Information System (INIS)

Ahmed, M.N.; Yasin, K.A.; Khan, R.A.H.; Mahmood, T.; Ayub, K.; Malik, D.

2017-01-01

Ethyl-6-(4-(ethoxycarbonyl)-1H-1,2,3-triazol-1-yl)pyridine-3-carboxylate (1), was synthesized via click reaction between ethyl tetrazolo[1,5-a]pyridine-6-carboxylate and ethyl propiolate in tetrahydrofuran (THF) in the presence of catalytic amount of a copper acetate. The structure was confirmed by single-crystal X-ray diffraction, NMR, FT-IR and MS. The compound crystallizes in the triclinic system, space group P-1 with a = 4.9122 (5), b = s9.5891 (11), c = 15.4851 (18) Å, a = 92.371 (5), beta = 90.015 (4), gamma = 101.722 (5) Z = 2 and V (Å /sup 3/) = 713.55 (14). Packing diagram indicates that there is dimeric interaction between two units via N(2)H(7). The crystal structure of the title compound 1 is stabilized by several nonboding interactions. Space filling model also revealed C-H...π and the π-π interactions in the molecule. Theoretical investigations were executed by using the Gaussian 09 software to enable comparison with X-ray structure as well as spectroscopic results, and to further probe the structural properties. The molecular electrostatic potential (MEP) analysis gave the idea about chemical reactivity and the Mulliken charge analysis gave quantitative estimate of the charges on the atoms. Frontier molecular orbitals analysis (electronic properties) was used to find the energy gap between the HOMO and the LUMO. The target compound was screened against three different bacterial strains like S. typhimurium, M. luteus and B. bronchiseptica as well as three different fungal strains i.e Aspergilus niger, Mucor specie and Aspergilus flavus. Moderate activities have been displayed by the target compound against tested strains. (author)

Crystal structure of 3-methyl-1-phenyl-5-(1H-pyrrol-1-yl-1H-pyrazole-4-carbaldehyde

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Joel T. Mague

2014-10-01

Full Text Available In the title compound, C15H13N3O, the pyrrolyl and phenyl rings make dihedral angles of 58.99 (5 and 34.95 (5°, respectively, with the central pyrazole ring. In the crystal, weak, pairwise C—H...O interactions across centers of symmetry form dimers, which are further associated into corrugated sheets running approximately parallel to (100 via weak C—H...N interactions.

Crystal structure, quantum mechanical investigation, IR and NMR spectroscopy of two new organic perchlorates: (C6H18N3)·(ClO4)3H2O (I) and (C9H11N2)·ClO4(II)

Science.gov (United States)

Bayar, I.; Khedhiri, L.; Soudani, S.; Lefebvre, F.; Ferretti, V.; Ben Nasr, C.

2018-06-01

The reaction of perchloric acid with 1-(2-aminoethyl)piperazine or 5,6-dimethyl-benzimidazole results in the formation of 1-(2-amonioethyl)piperazine-1,4-dium triperchlorate hydrate (C6H18N3)·(ClO4)3·H2O (I) or 5,6-dimethyl-benzylimidazolium perchlorate (C9H11N2)·ClO4(II). Both compounds were fully structurally characterized including single crystal X-ray diffraction analysis. Compound (I) crystallizes in the centrosymmetric triclinic space group P 1 bar with the lattice parameters a = 7.455 (2), b = 10.462 (2), c = 10.824 (2) Å, α = 80.832 (2), β = 88.243 (2), γ = 88.160 (2) °, Z = 2 and V = 832.77 (3) Å3. Compound (II) has been found to belong to the P21/c space group of the monoclinic system, with a = 7.590 (3), b = 9.266 (3), c = 16.503 (6) Å, β = 107.38 (2) °, V = 1107.69 (7) Å3 and Z = 4. The structures of (I) and (II) consist of slightly distorted [ClO4]- tetrahedra anions and 1-(2-amonioethyl)piperazine-1,4-dium trication (I) or 5,6-dimethyl-benzylimidazolium cations (II) and additionally a lattice water in (I). The crystal structures of (I) and (II) exhibit complex three-dimensional networks of H-bonds connecting all their components. In the atomic arrangement of (I), the ClO4- anions form corrugated chains, while in (II) the atomic arrangement exhibits wide pseudo-hexagonal channels of ClO4 tetrahedra including the organic entities. The lattice water serves as a link between pairs of cations and pairs of anions via several Osbnd H⋯O and N-H⋯O interactions in compound (I). The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13C, 35Cl and 15N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands. Intermolecular interactions were investigated by Hirshfeld surfaces. Electronic properties such as HOMO and LUMO energies were derived.

Methyl (9aR*,10S*,11R*,13aS*,13bS*-9-oxo-6,7,9,9a,10,11-hexahydro-5H,13bH-11,13a-epoxypyrrolo[2′,1′:3,4][1,4]diazepino[2,1-a]isoindole-10-carboxylate

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Flavien A. A. Toze

2011-11-01

Full Text Available The title compound, C17H18N2O4, is the methyl ester of the adduct of intramolecular Diels–Alder reaction between maleic anhydride and 1-(2-furyl-2,3,4,5-tetrahydro-1H-pyrrolo[1,2-a][1,4]diazepine. The molecule comprises a fused pentacyclic system containing four five-membered rings (viz. pyrrole, 2-pyrrolidinone, tetrahydrofuran and dihydrofuran and one seven-membered ring (1,4-diazepane. The pyrrole ring is approximately planar (r.m.s. deviation = 0.003 Å while the 2-pyrrolidinone, tetrahydrofuran and dihydrofuran five-membered rings have the usual envelope conformations. The central seven-membered diazepane ring adopts a boat conformation. In the crystal, molecules are bound by weak intermolecular C—H...O hydrogen-bonding interactions into zigzag chains propagating in [010]. In the crystal packing, the chains are stacked along the a axis.

Synthesis of both sup 14 C- and sup 3 H- labelled trospectomycin and the assessment of their utility in biological studies

Energy Technology Data Exchange (ETDEWEB)

Constable, D A; Dring, L G [Upjohn Ltd., Crawley (UK); Jones, J R [Surrey Univ., Guildford (UK). Dept. of Chemistry

1990-07-01

Three radiolabelled forms of trospectomycin (6'-n-propylspectinomycin sulphate hydrate) have been synthesised, namely (8'-{sup 14}C)-, (6',7'-{sup 3}H)-, and (5',6',7'-{sup 3}H)-trospectomycin. Although all three forms of the drug are metabolically stable and therefore suitable for use in animal studies the {sup 14}C compound is produced in poor yield as is the (6',7'-{sup 3}H)trospectomycin. On the other hand, the (5',6',7'-{sup 3}H)-form is produced in good yield and appears to be the labelled form of choice. Following subcutaneous administration of any of the labelled forms to rats, more than 50% of the dose was excreted in the urine as unchanged drug during the first 6h after dosing. Approximately 80% and 10% of the dose appeared in the urine and faeces respectively after 6 days. (author).

catena-Poly[[[aquasilver(I]-μ-1,1′-(butane-1,4-diyldi-1H-imidazole-κ2N3:N3′] hemi(biphenyl-4,4′-dicarboxylate dihydrate

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Zheyu Zhang

2009-12-01

Full Text Available In the title compound, {[Ag(C10H14N4(H2O](C14H8O40.5·2H2O}n, the AgI ion is three-coordinated by two N atoms from two independent 1,1′-(butane-1,4-diyldi-1H-imidazole (BBI ligands and one water O atom in a distorted T-shaped coordination geometry. The biphenyl-4,4′-dicarboxylate (BPDC dianions do not coordinate to AgI ions but act as counter-ions. The AgI ions are linked by BBI ligands, forming a zigzag chain. These chains are linked into a two-dimensional supramolecular architecture by O—H...O hydrogen-bonding interactions between water molecules and carboxylate O atoms of the BPDC dianions.

Triosmium cluster compounds containing isocyanide and hydride ligands. Crystal and molecular structure of (μ-H)(μ-eta1-C==N(H)(t-C4H9))Os3(CO)10

International Nuclear Information System (INIS)

Adams, R.D.; Golembeski, N.M.

1979-01-01

The crystal and molecular structure of the compound (μ-H)(μ-eta 1 -C==N(H)(t-C 4 H 9 ))Os 3 (CO) 10 has been determined by X-ray crystallographic methods. The compound crystallizes in the centrosymmetric monoclinic space group P2 1 /n[C/sub 2h/ 5 ]:a = 13.651 (4) A, b = 9.156 (4) A, c = 18.275 (5) A, β = 111.42 (2) 0 , V = 2126.3 (25) A 3 , Z = 4, rho/sub calcd/ = 2.92 g cm -3 . A uniform triangular cluster of three osmium atoms contains ten linear carbonyl groups and a μ-eta 1 -C==N(H)(t-C 4 H 9 ) iminyl ligand. The carbon atom of the iminyl ligand symmetrically bridges one osmium-osmium bond, as is shown by the internuclear separations Os(2)-C(11) = 2.066 (8) A and Os(3)-C(11) = 2.043 (8) A. The iminyl bond, C(11)-N, is double with the C-N distance being 1.298 (10) A

(1-Phenyl-1H-1,2,3-triazol-4-ylmethyl pyridine-3-carboxylate

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Zakirjon Karimov

2010-07-01

Full Text Available In the title compound, C15H12N4O2, the dihedral angle between the planes of the nicotinoyloxy fragment and triazole ring is 88.61 (5°. The dihedral angle between the planes of triazole and benzene rings is 16.54 (11°. The crystal structure is stabilized by intermolecular C—H...N, C—H...O and C—H...π(triazole hydrogen bonds and aromatic π–π stacking interactions between the benzene and triazole rings [centroid–centroid distance = 3.895 (1 Å

(E-3-Methyl-6-(3-oxo-3-(3,4,5-trimethoxyphenylprop-1-en-1-yl-2(3H-benzothiazolone

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Yordanka Ivanova

2016-09-01

Full Text Available The title compound, (E-3-methyl-6-(3-oxo-3-(3,4,5-trimethoxyphenylprop-1-en-1-yl-2(3H-benzothiazolone, was synthesized by both an acid- and base-catalyzed aldol condensation of 3-methyl-6-acetyl-2(3H-benzothiazolone and 3,4,5-trimethoxyacetophenone. The structure of the target compound was confirmed using 1H-NMR, 13C-NMR, IR, MS, and elemental analysis.

1-Propyl-1H-indole-2,3-dione

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Fatima Zahrae Qachchachi

2016-04-01

Full Text Available In the title compound, C11H11NO2, the 1H-indole-2,3-dione unit is essentially planar, with an r.m.s. deviation of 0.0387 (13 Å. This plane makes a dihedral angle of 72.19 (17° with the plane of the propyl substituent. In the crystal, chains propagating along the b axis are formed through C—H...O hydrogen bonds.

Synthesis of [3-14C]- and [phenyl-U-14C] olaquindox

International Nuclear Information System (INIS)

Maul, W.; Scherling, D.; Seng, F.

1981-01-01

Olaquindox is a new feed additive. [ 14 C]Olaquindox, labelled in different positions, was needed for tracer-studies of pharmacokinetics, biotransformation and residues in several species of animals. 2-[N-(2-hydroxethyl)-carbamoyl]-3-methyl-[3- 14 C]quinoxaline-1,4-dioxide([3- 14 C]Olaquindox) was synthesized from barium[ 14 C]carbonate (22 mmoles; 1.15 Ci) via [1- 14 C]acetic acid, sodium[1- 14 C]acetate, [1- 14 C]acetylchloride, ethyl[3- 14 C]acetoacetate and 2-carbethoxy-3-methyl-[3- 14 C]quinoxaline-1,4-dioxide with an overall yield of 10%, based on barium[ 14 C]carbonate. The radiochemical purity was better than 98% (tlc). The specific activities of three preparations were 10.5, 8.4 and 5.45 μCi/mg respectively. [phenyl-U- 14 C]Olaquindox was synthesized starting from [U- 14 C]aniline (19.8 mmoles; 284.4 mCi). Intermediate products were N-acetyl[U- 14 C]aniline, 2-nitro-N-acetyl[U- 14 C]aniline, 2-nitro[U- 14 C]aniline and [U- 14 C]benzofurazanoxide. The total yield was 50% as calculated for [U- 14 C]aniline. At calibration samples of two preparations showed specific activities of 49.5 and 11.1 μCi/mg respectively. The radiochemical purity was checked by tlc and exceeded 98%. (author)

(R,S-2′-Amino-6′-methyl-2,5′,5′-trioxo-6′H-spiro[indoline-3,4′-pyrano[3,2-c][2,1]benzothiazine]-3′-carbonitrile dimethylformamide monosolvate

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Svitlana V. Shishkina

2014-07-01

Full Text Available The title solvate, C20H14N4O4S·C3H7NO, comprises a stereogenic centre but the centrosymmetric space group causes the presence of the racemate in the crystal. The spiro-joined fragments are almost orthogonal, with a dihedral angle of 86.8 (2° between the mean planes of the pyrane ring and the dihydroindolone ring system. The atoms of the indolinone bicycle are coplanar, with an r.m.s. deviation of 0.005 Å. In the crystal, pairs of N—H...O hydrogen bonds link the molecules into centrosymmetric dimers which are linked to the dimethylformamide solvent molecules by further N—H...O hydrogen bonds. N—H...N hydrogen bonds link neighbouring dimers into [010] chains.

[2,3,7,8,13,14,17,18-Octa-kis(ethyl-sulfan-yl)-5,10,15,20-porphyrazinato]zinc(II).

Science.gov (United States)

Akkurt, Mehmet; Coşkun, Naciye Yılmaz; Kılıçaslan, Fatma Aytan; Yalçın, Sabiha Manav; Büyükgüngör, Orhan; Gül, Ahmet

2010-07-24

In the title compound, [Zn(C(32)H(40)N(8)S(8))], the Zn(II) ion is coordinated by four N atoms in a slightly distorted square-planar environment. In addition, there is a Zn⋯S contact involving a symmetry-related S atom which, when considered, forms a pseudo-square-pyramidal coordination with respect to the Zn(II) ion. Three of the ethyl groups are disordered over two sites with occupancy ratios of 0.841 (10):0.159 (10), 0.802 (10):0.198 (10) and 0.457 (13):0.543 (13). Weak intra-molecular C-H⋯N and C-H⋯S inter-actions contribute to the stability of the mol-ecular conformation. Inter-molecular C-H⋯S contacts, weak C-H⋯π inter-actions and π-π stacking inter-actions [centroid-centriod distances = 3.832 (4) and 3.850 (5) Å] contribute to the stabilization of the crystal structure.

(1S,3S,8R,9S,10R-9,10-Epoxy-3,7,7,10-tetramethyltricyclo[6.4.0.01,3]dodecane

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Abdoullah Bimoussa

2014-04-01

Full Text Available The title compound, C16H26O, was synthesized by treating (1S,3S,8R-3,7,7,10-tetramethyltricyclo[6.4.0.01,3]dodec-9-ene with metachloroperbenzoic acid. The molecule is built up from two fused six- and seven-membered rings. The six-membered ring has a half-chair conformation, whereas the seven-membered ring displays a boat conformation. In the crystal, there are no significant intermolecular interactions present.

1,5-Bis (2-Hydroxyphenyl)Pent-1,4-Diene-3-One: A Lead ...

African Journals Online (AJOL)

NJD

occurring chalcone nucleus to design effective antibacterial agents. The present investigation established 1,5-bis(2-hydroxyphenyl)pent-1,4-diene-3-one (1c) as a lead compound with potential against a panel of pathogenic bacterial strains, ...

Crystal structure of 2-[(3aS,6R-3,3,6-trimethyl-3,3a,4,5,6,7-hexahydro-2H-indazol-2-yl]thiazol-4(5H-one

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Abdellah N'ait Ousidi

2016-03-01

Full Text Available The title compound, C13H19N3OS, is a new thiazolidin-4-one derivative prepared and isolated as the pure (3aS,6R-diastereisomer from (R-thiosemicarbazone pulegone. It crystallized with two independent molecules (A and B in the asymmetric unit. The compound is composed of a hexhydroindazole ring system (viz. a five-membered dihydropyrazole ring fused to a cyclohexyl ring with a thiazole-4-one ring system attached to one of the pyrazole N atoms (at position 2. The overall geometry of the two molecules differs slightly, with the mean planes of the pyrazole and thiazole rings being inclined to one another by 10.4 (1° in molecule A and 0.9 (1° in molecule B. In the crystal, the A and B molecules are linked via C—H...O hydrogen bonds, forming slabs parallel to the ab plane. There are C—H...π interactions present within the layers, and between the layers, so forming a three-dimensional structure.

Propyl 3-oxo-2,3-dihydro-1,2-benzothia-zole-2-carboxyl-ate.

Science.gov (United States)

Wang, Xiang-Hui; Yang, Jian-Xin; You, Cheng-Hang; Lin, Qiang

2011-09-01

The title compound, C(11)H(11)NO(3)S, was synthesized by the reaction of benzo[d]isothia-zol-3(2H)-one with propyl carbono-chloridate in toluene. The benzoisothiazolone ring system is approximately planar with a maximum deviation from the mean plane of 0.0226 (14) Å for the N atom. Weak inter-molecular C-H⋯O hydrogen bonding occurs in the crystal structure.

Rietveld refinement of the structures of 1.0 C-S-H and 1.5 C-S-H

KAUST Repository

Battocchio, Francesco

2012-11-01

Low-Q region Rietveld analyses were performed on C-S-H synchrotron XRD patterns, using the software MAUD. Two different crystal structures of tobermorite 11 Å were used as a starting model: monoclinic ordered Merlino tobermorite, and orthorhombic disordered Hamid tobermorite. Structural modifications were required to adapt the structures to the chemical composition and the different interlayer spacing of the C-S-H samples. Refinement of atomic positions was done by using special constraints called fragments that maintain interatomic distances and orientations within atomic polyhedra. Anisotropic crystallite size refinement showed that C-S-H has a nanocrystalline disordered structure with a preferred direction of elongation of the nanocrystallites in the plane of the Ca interlayer. The quality of the fit showed that the monoclinic structure gives a more adequate representation of C-S-H, whereas the disordered orthorhombic structure can be considered a more realistic model if the lack of long-range order of the silica chain along the c-direction is assumed. © 2012 Elsevier Ltd. All rights reserved.

1,3-Dimethyl-1H-indole-2-carbonitrile

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Jiang-Sheng Li

2009-08-01

Full Text Available The title compound, C11H10N2, crystallizes with two molecules in the asymmetric unit, both of which are essentially planar (r.m.s. deviations = 0.014 and 0.016 Å. In the crystal, aromatic π–π stacking interactions occur [shortest centroid–centroid separation = 3.5569 (11 Å].

Dicyclohexylammonium (S-2-azido-3-phenylpropanoate

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Sebastian J. Petrik

2012-07-01

Full Text Available The asymmetric unit of the title compound, C12H24N+·C9H8N3O2−, consists of two dicyclohexylammonium cations linked to two (S-2-azido-3-phenylpropanoate anions by four short N—H...O hydrogen bonds with N...O distances in the range 2.712 (3–2.765 (3 Å. The dicyclohexylammonium cations and the aryl and carboxylate groups of the anion are related by a pseudo-inversion centre, with overall crystallographic inversion symmetry for the structure broken by the chirality of the α-C atoms of the anions.

(11-Methylpyrido[2,3-b][1,4]benzodiazepin-6-yl(phenylmethanone

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Fuqiang Shi

2010-09-01

Full Text Available In the title compound, C20H15N3O, the diazepine ring adopts a boat conformation. The dihedral angle between pyridine and benzene rings is 55.2 (1°. The benzoyl phenyl ring forms dihedral angles of 49.4 (1 and 75.9 (1°, respectively, with the pyridine and benzene rings. In the crystal, molecules are linked into centrosymmetric dimers by pairs of C—H...N hydrogen bonds.

Tert-butyl 3-oxo-2,3,4,5,6,7-hexahydro-1H-pyrazolo[4,3-c]pyridine-5-carboxylate

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Tara Shahani

2010-01-01

Full Text Available In the title compound, C11H17N3O3, the pyrazole ring is approximately planar, with a maximum deviation of 0.005 (2 Å, and forms a dihedral angle of 5.69 (13° with the plane through the six atoms of the piperidine ring. In the crystal, pairs of intermolecular N—H...O hydrogen bonds form dimers with neighbouring molecules, generating R22(8 ring motifs. These dimers are further linked into two-dimensional arrays parallel to the bc plane by intermolecular N—H...O and C—H...O hydrogen bonds.

Synthesis, X-ray Single Crystal Structure, Molecular Docking and DFT Computations on N-[(1E)-1-(2H-1,3-Benzodioxol-5-yl)-3-(1H-imidazol-1-yl)propylidene]-hydroxylamine: A New Potential Antifungal Agent Precursor.

Science.gov (United States)

Al-Wabli, Reem I; Al-Ghamdi, Alwah R; Ghabbour, Hazem A; Al-Agamy, Mohamed H; Monicka, James Clemy; Joe, Issac Hubert; Attia, Mohamed I

2017-02-28

Mycoses are serious health problem, especially in immunocompromised individuals. A new imidazole-bearing compound containing an oxime functionality was synthesized and characterized with different spectroscopic techniques to be used for the preparation of new antifungal agents. The stereochemistry of the oxime double bond was unequivocally determined via the single crystal X-ray technique. The title compound 4 , C 13 H 13 N₃O₃·C₃H₈O, crystallizes in the monoclinic space group P 2₁with a = 9.0963(3) Å, b = 14.7244(6) Å, c = 10.7035(4) Å, β = 94.298 (3)°, V = 1429.57(9) ų, Z = 2. The molecules were packed in the crystal structure by eight intermolecular hydrogen bond interactions. A comprehensive spectral analysis of the title molecule 4 has been performed based on the scaled quantum mechanical (SQM) force field obtained by density-functional theory (DFT) calculations. A molecular docking study illustrated the binding mode of the title compound 4 into its target protein. The preliminary antifungal activity of the title compound 4 was determined using a broth microdilution assay.

Crystal structure of 1-{4-hydroxy-3-[(pyrrolidin-1-ylmethyl]phenyl}-3-phenylprop-2-en-1-one

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Abdullah Aydın

2016-05-01

Full Text Available In the title compound, C20H21NO2, the pyrrolidine ring adopts an envelope conformation with the N atom at the flap position. The central benzene ring makes dihedral angles of 21.39 (10 and 80.10 (15° with the phenyl ring and the mean plane of the pyrrolidine ring, respectively. The molecular conformation is stabilized by an intramolecular O—H...N hydrogen bond, which closes an S(6 ring. A weak C—H...π interaction is observed in the crystal.

1,4,9,12-Tetramethoxy-14-octyl-5,8-dihydrodiindolo[3,2-b;2′,3′-h]carbazole with an unknown solvent

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Norma Wrobel

2017-03-01

Full Text Available The title compound, 2C36H39N3O4·H2O, is a linear π-conjugated ladder oligomer with an alkyl chain on the central nitrogen atom. This diindolocarbazole, prepared via a twofold Cadogan reaction, adopts a sligthly convex shape, anti to the disordered octyl group. The unit cell contains nine molecules of the title compound and half a water molecule per main molecule. The water molecule forms hydrogen bridges, connecting the carbazole-NH and methoxy groups of different molecules. The crystal contains solvent molecules which are located in a channel parallel to the c axis. It was not possible to determine the position and nature of the solvent (a mixure of choroform, n-pentane and DMSO. The SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] option of PLATON was used to model the missing electron density. The given chemical formula and other crystal data do not take into account these solvent molecules.

Synthesis and Molecular Structure of 6-Amino-3-benzylmercapto-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one

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Gene-Hsiang Lee

2006-03-01

Full Text Available The title compound 6-amino-3-benzylmercapto-1,2,4-triazolo[3,4-f][1,2,4]-triazin-8(7H-one (4, molecular formula C11H10N6OS, was obtained by the reaction of3-amino-2-benzyl-6-hydrazino-1,2,4-triazin-5(2H-one (3 with carbon disulfide in awater/pyridine mixture. Compound 4 can also be synthesized by reacting6-amino-3(2Hmercapto-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one (7 with benzylbromide in methanolic ammonia water. The compound crystallizes in the monoclinicspace group P21/c with a = 7.2926(15, b = 14.456(2, c = 11.436(2 å, β = 105.30(2°, V= 1162.9(4 å3 and Z = 4, resulting in a density Dcalc of 1.567 g/cm3. Molecules of 4 arelinked by extensive intermolecular N-H···N and N-H···O hydrogen bonding [graph set R22 (9]. The structure is further stabilized by π-π stacking interactions. 2

Crystal structure of 1-ethylpyrazolo[3,4-d]pyrimidine-4(5H-thione

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Mohammed El Fal

2014-09-01

Full Text Available In the title compound, C7H8N4S, the methyl C atom is displaced by 1.232 (7 Å from the mean plane of the pyrazolo[3,4-d]pyrimidine ring system (r.m.s. deviation = 0.007 Å. The N—N—C—Cm (m = methyl torsion angle is −60.3 (6°. In the crystal, molecules are linked by N—H...S hydrogen bonds, generating [010] chains, which are reinforced by C—H...N interactions. The chains are cross-linked by weak C—H...S hydrogen bonds, generating (001 sheets.

Crystal structure of (2R*,3aR*-2-phenylsulfonyl-2,3,3a,4,5,6-hexahydropyrrolo[1,2-b]isoxazole

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Yaiza Hernández

2017-01-01

Full Text Available The title compound, C12H15NO3S, was prepared by 1,3-dipolar cycloaddition of 3,4-dihydro-2H-pyrrole 1-oxide and phenyl vinyl sulfone. In the molecule, both fused five-membered rings display a twisted conformation. In the crystal, C—H...O hydrogen bonds link neighbouring molecules, forming chains running parallel to the b axis.

Dipropyl 3,6-diphenyl-1,2-dihydro-1,2,4,5-tetrazine-1,2-dicarboxylate.

Science.gov (United States)

Rao, Guo-Wu; Hu, Wei-Xiao

2003-05-01

The title compound, C(22)H(24)N(4)O(4), was prepared from propyl chloroformate and 3,6-diphenyl-1,2-dihydro-s-tetrazine. This reaction yields the title compound rather than dipropyl 3,6-diphenyl-1,4-dihydro-s-tetrazine-1,4-dicarboxylate. The 2,3-diazabutadiene group in the central six-membered ring is not planar; the C=N double-bond length is 1.285 (2) A, and the average N-N single-bond length is 1.401 (3) A, indicating a lack of conjugation. The ring has a twist conformation, in which adjacent N atoms lie +/- 0.3268 (17) A from the plane of the ring. The molecule has twofold crystallographic symmetry.

(2S,4R-2-[(1R-1-(4-Bromophenyl-2-nitroethyl]-4-ethylcyclohexanone

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Chi-Xiao Zhang

2013-02-01

Full Text Available The crystal structure of the title compound, C16H20BrNO3, contains three chiral centers in the configuration 1R,2S,6R. The cyclohexane ring is in a chair conformation. In the crystal, molecules are linked by weak C—H...O interactions, forming chains along the a-axis direction.

The 14-3-3 protein interacts directly with the C-terminal region of the plant plasma membrane H(+)-ATPase

DEFF Research Database (Denmark)

Jahn, T.; Fuglsang, A.T.; Olsson, A.

1997-01-01

Accumulating evidence suggests that 14-3-3 proteins are involved in the regulation of plant plasma membrane H(+)-ATPase activity. However, it is not known whether the 14-3-3 protein interacts directly or indirectly with the H(+)-ATPase. In this study, detergent-solubilized plasma membrane H...... plasma membrane H(+)-ATPase. We propose that the 14-3-3 protein is a natural ligand of the plasma membrane H(+)-ATPase, regulating proton pumping by displacing the C-terminal autoinhibitory domain of the H(+)-ATPase....

11 CFR 100.14 - State committee, subordinate committee, district, or local committee (2 U.S.C. 431(15)).

Science.gov (United States)

2010-01-01

... 11 Federal Elections 1 2010-01-01 2010-01-01 false State committee, subordinate committee, district, or local committee (2 U.S.C. 431(15)). 100.14 Section 100.14 Federal Elections FEDERAL ELECTION COMMISSION GENERAL SCOPE AND DEFINITIONS (2 U.S.C. 431) General Definitions § 100.14 State committee...

2-Hydroxy-16-[(E-4-methylbenzylidene]-13-(4-methylphenyl-12-phenyl-1,11-diazapentacyclo[12.3.1.02,10.03,8.010,14]octadeca-3(8,4,6-triene-9,15-dione

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Raju Suresh Kumar

2010-08-01

Full Text Available In the title compound, C37H32N2O3, an intramolecular O—H...N hydrogen bond generates a five-membered ring, producing an S(5 motif. The piperidone ring adopts a half-chair conformation. The two fused pyrrolidine rings have similar envelope conformations. The interplanar angles between the benzene rings A/B and C/D are 75.68 (7 and 30.22 (6°, respectively. In the crystal structure, adjacent molecules are interconnected into chains propagating along the [010] direction via intermolecular C—H...O hydrogen bonds. Further stabilization is provided by weak C—H...π interactions.

Three closely related 4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridines: synthesis, molecular conformations and hydrogen bonding in zero, one and two dimensions.

Science.gov (United States)

Sagar, Belakavadi K; Harsha, Kachigere B; Yathirajan, Hemmige S; Rangappa, Kanchugarakoppal S; Rathore, Ravindranath S; Glidewell, Christopher

2017-03-01

In each of 1-(4-fluorophenyl)-5-methylsulfonyl-3-[4-(trifluoromethyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine, C 21 H 19 F 4 N 3 O 2 S, (I), 1-(4-chlorophenyl)-5-methylsulfonyl-3-[4-(trifluoromethyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine, C 21 H 19 ClF 3 N 3 O 2 S, (II), and 1-(3-methylphenyl)-5-methylsulfonyl-3-[4-(trifluoromethyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine, C 22 H 22 F 3 N 3 O 2 S, (III), the reduced pyridine ring adopts a half-chair conformation with the methylsulfonyl substituent occupying an equatorial site. Although compounds (I) and (II) are not isostructural, having the space groups Pbca and P2 1 2 1 2 1 , respectively, their molecular conformations are very similar, but the conformation of compound (III) differs from those of (I) and (II) in the relative orientation of the N-benzyl and methylsulfonyl substituents. In compounds (II) and (III), but not in (I), the trifluoromethyl groups are disordered over two sets of atomic sites. Molecules of (I) are linked into centrosymmetric dimers by C-H...π(arene) hydrogen bonds, molecules of (II) are linked by two C-H...O hydrogen bonds to form ribbons of R 3 3 (18) rings, which are themselves further linked by a C-Cl...π(arene) interaction, and a combination of C-H...O and C-H...π(arene) hydrogen bonds links the molecules of (III) into sheets. Comparisons are made with the structures of some related compounds.

Spread-F occurrences and relationships with foF2 and h'F at low- and mid-latitudes in China

Science.gov (United States)

Wang, Ning; Guo, Lixin; Zhao, Zhenwei; Ding, Zonghua; Lin, Leke

2018-04-01

Ionospheric irregularities are an important phenomenon in scientific studies and applications of radio-wave propagation. Spread-F echoes in ionograms are a type of high-frequency band irregularities that include frequency spread-F (FSF), range spread-F (RSF), and mixed spread-F (MSF) events. In this study, we obtained spread-F data from four ionosondes at low- and mid-latitudes near the 120°E chain in China during the 23rd solar cycle. We used these data to investigate spread-F occurrence percentages and variations with local time, season, latitude, and solar activity. The four ionosondes were located at Haikou (HK) (20°N, 110.34°E), Guangzhou (GZ) (23.14°N, 113.36°E), Beijing (BJ) (40.11°N, 116.28°E), and Changchun (CC) (43.84°N, 125.28°E). We also present possible correlations between spread-Fs and other ionospheric parameters, such as the critical frequency of the F2-layer (foF2) and the virtual height of the bottom-side F-layer (h'F). In particular, we investigated the possible threshold of the foF2 affecting the FSF and the relationship between the h'F and the RSF. The main conclusions are as follows: (a) the FSF occurrence percentages were anti-correlated with solar activity at all four sites; meanwhile, RSF occurrence rates increased with the increase in solar activity at HK, but not at the other three sites; (b) FSF occurrence rates were larger at the mid-latitudes than expected, while FSFs occurred more often after midnight; (c) the highest FSF occurrence rates mostly appeared during the summer months, while RSFs occurred mostly in the equinoctial months of 2000-2002 at HK and GZ; (d) a lower foF2 was suitable for FSF events; nevertheless, h'F and RSF occurrences satisfied the parabolic relationship; (e) the foF2 thresholds for FSFs were 15, 14, 7.6, and 7.8 MHz at HK, GZ, BJ, and CC, respectively. The h'Fs occurring between 240 and 290 km were more favorable for RSF occurrences. These results are important for understanding ionospheric

Crystal structure and Hirshfeld surface analysis of (2E,2′E-3,3′-(1,4-phenylenebis[1-(2,4-difluorophenylprop-2-en-1-one

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Huey Chong Kwong

2017-12-01

Full Text Available The asymmetric unit of the title compound, C24H14F4O2, comprises of one and a half molecules; the half-molecule is completed by crystallographic inversion symmetry. In the crystal, molecules are linked into a three-dimensional network by C—H...F and C—H...O hydrogen bonds. Some of the C—H...F links are unusually short (< 2.20 Å. Hirshfeld surface analyses (dnorm surfaces and two-dimensional fingerprint plots for the title compound are presented and discussed.

ANTI-ALLERGIC EFFECTS OF 1,5-BIS(4’-HYDROXY-3’-METHOXYPHENYL-1,4-PENTADIENE-3-ONE ON MAST CELL-MEDIATED ALLERGY MODEL

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AGUNG ENDRO NUGROHO

2009-01-01

Full Text Available 1,5-bis(4’-hydroxy-3’-methoxyphenyl-1,4-pentadiene-3-one is a 1,5-diphenyl-1,4-pentadiene-3-one analogue of curcumin that is produced by modifying the middle site of curcumin leading to 1,4-pentadiene-3-ones to maintain the hydroxy moiety at the aromatic rings that are responsible for its biological activities. Curcumin has been reported to have anti-allergic effects and can inhibit the release of histamine from mast cells. In the present study, we evaluated the anti-allergic effects of 1,5-bis(4’-hydroxy-3’-methoxyphenyl-1,4-pentadiene-3-one in a mast cell-mediated allergy mode in order to provide information about a newly synthesised-compound for an alternative allergy drug. The study was performed using (1 a rat basophilic leukaemia (RBL-2H3 cell line, which is a tumour analogue of mast cells, with DNP24-BSA, thapsigargin and ionomycin as inducers for secretory markers from mast cells, and (2 an active cutaneous anaphylaxis (ACA reaction, with ovalbumin as an inductor of mast cell degranulation. Treatment with 1,5-bis(4’-hydroxy-3’-methoxyphenyl-1,4-pentadiene-3-one strongly inhibited the DNP24-BSA, thapsigargin and ionomycin-mediated release of histamine and β-hexosaminidase from the RBL-2H3 cell line. The results indicated that this compound influenced the activation processes of FcεRI by antigen and intracellular Ca2+ signalling events in mast cells. In type 1 allergy model, this compound also inhibited the active cutaneous anaphylactic reaction on rat dorsal skins generated by ovalbumin. We conclude that the compound 1,5-bis(4’-hydroxy-3’-methoxyphenyl-1,4-pentadiene-3-one showed anti-allergic activities mediated by mechanisms related to intracellular signalling events in mast cells.

(3R,5S,7R,8R,9S,10S,12S,13R,14S-10,13-Dimethyl-17-[5-oxo-5-(prop-2-yn-1-yloxypentan-2-yl]hexadecahydro-1H-cyclopenta[a]phenanthrene-3,7,12-triyl triacetate

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T. Kavitha

2017-03-01

Full Text Available In the title compound, C33H48O8, four terminal H atoms of cholic acid are replaced by three acetyl and one terminal alkyne group. All the acetyl residues are twisted with respect to the rings (A, B and C to which they are attached. The cyclopentane ring D adopts an envelope conformation with the methyl-substituted C atom as the flap. Rings A, B and C have chair conformations. The dihedral angle between the mean planes of rings C and D is 4.70 (11°. In the crystal, molecules are linked by C—H...O hydrogen bonds, forming a three-dimensional structure.

N-(4-Methoxyphenyl-4-methylbenzenesulfonamide

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Islam Ullah Khan

2011-01-01

Full Text Available In the title compound, C14H15NO3S, the dihedral angle between the aromatic rings is 59.39 (14° and the C—S—N—C torsion angle is −71.4 (2°. In the crystal, a supramolecular chain running along the b axis with a C(4 graph set is formed via N—H...O hydrogen bonds.

(2RS-2-(2,4-Difluorophenyl-1-[(4-iodobenzyl(methylamino]-3-(1H-1,2,4-triazol-1-ylpropan-2-ol

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Hui-Ping Xiong

2012-08-01

Full Text Available In the title compound (common name: iodiconazole, C19H19F2IN4O, there is an intramolecular O—H...N hydrogen bond and molecules are linked by weak interactions only, namely C—H...N, C—H...O and C—H...F hydrogen bonds, and π-electron ring–π-electron ring interactions between the triazole rings with centroid–centroid distances of 3.725 (3 Å.

Crystal structure of 3-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacen-3-ylpropanoic acid

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Takuma Kato

2017-12-01

Full Text Available The crystal structure of the title compound, C14H15BF2N2O2, which comprises a boron–dipyrromethene (BODIPY backbone and a propionic acid group, has been determined at 100 K. The BODIPY fused-ring system is nearly planar, with a maximum deviation from the mean plane of 0.032 (2 Å. In the crystal, pairs of O—H...O hydrogen bonds connect the molecules, forming inversion dimers. The dimers are linked via C—H...O hydrogen bonds, forming a tape along the a axis. The tapes are stacked along the c axis through C—H...F hydrogen bonds and π–π interactions.

5-Isobutyl-4-phenylsulfonyl-1H-pyrazol-3(2H-one

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M. Venkatesh

2010-12-01

Full Text Available The title compound, C13H16N2O3S, consists of two crystallographically independent molecules with similar geometries and exists in a keto form, the C=O bond lengths being 1.267 (2 and 1.254 (2 Å. In both molecules, the pyrazole rings are approximately planar, with maximum deviations of 0.017 (2 and 0.010 (2 Å, and the dihedral angles between the pyrazole and phenyl rings are 83.63 (11 and 70.07 (12°. In one molecule, an intramolecular C—H...O hydrogen bond with an S(6 ring motif is observed. In the crystal, intermolecular N—H...O and C—H...O hydrogen bonds link the molecules into two-dimensional networks parallel to the ab plane.

N-(4-Nitrobenzoyl)-N'-(1,5-dimethyl-3-oxo-2-phenyl-1H-3(2H)-pyrazolyl)-thiourea hydrate: Synthesis, spectroscopic characterization, X-ray structure and DFT studies

Science.gov (United States)

Arslan, N. Burcu; Kazak, Canan; Aydın, Fatma

2012-04-01

The title molecule (C19H17N5O4S·H2O) was synthesized and characterized by IR-NMR spectroscopy, MS and single-crystal X-ray diffraction. The molecular geometry, vibrational frequencies and gauge-independent atomic orbital (GIAO) 1H and 13C NMR chemical shift values of the compound in the ground state have been calculated by using the density functional theory (DFT) method with 6-31G(d) basis set, and compared with the experimental data. All the assignments of the theoretical frequencies were performed by potential energy distributions using VEDA 4 program. The calculated results show that the optimized geometries can well reproduce the crystal structural parameters, and the theoretical vibrational frequencies and 1H and 13C NMR chemical shift values show good agreement with experimental data. To determine conformational flexibility, the molecular energy profile of the title compound was obtained with respect to the selected torsion angle, which was varied from -180° to +180° in steps of 10°. Besides, molecular electrostatic potential (MEP), frontier molecular orbitals (FMO) analysis and thermodynamic properties of the compound were investigated by theoretical calculations.

2-(2,4-Dichlorophenyl-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylacetamide

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B. Narayana

2013-01-01

Full Text Available In the crystal structure of the title compound, C19H17Cl2N3O2, the molecules form dimers of the R22(10 type through N—H...O hydrogen bonding. As a result of steric repulsion, the amide group is rotated with respect to both the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings, making dihedral angles of 80.70 (13 and 64.82 (12°, respectively. The dihedral angle between the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings is 48.45 (5° while that between the 2,3-dihydro-1H-pyrazol-4-yl and phenyl rings is 56.33 (6°.

Synthesis, Crystal Structure, DFT Study and Antifungal Activity of 4-(5-((4-Bromobenzyl thio-4-Phenyl-4H-1,2,4-Triazol-3-ylpyridine

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Jin-Xia Mu

2015-12-01

Full Text Available The title compound 4-(5-((4-bromobenzylthio-4-phenyl-4H-1,2,4-triazol-3-ylpyridine (C20H15BrN4S was synthesized, and its structure was confirmed by 1H NMR, MS and elemental analyses and single-crystal X-ray structure determination. It crystallizes in the triclinic space group P-1 with a = 7.717(3, b = 9.210(3, c = 13.370(5 Å, α = 80.347(13, β = 77.471(13, γ = 89.899(16°, V = 913.9(6 Å3, Z = 2 and R = 0.0260 for 3145 observed reflections with I > 2σ(I. A Density functional theory (DFT (B3LYP/6-31G calculation of the title molecule was carried out. The full geometry optimization was carried out using a 6-31G basis set, and the frontier orbital energy. Atomic net charges are discussed. Calculated bond lengths and bond angles were found to differ from experimental values, and the compound exhibits moderate antifungal activity.

(2Z,2′Z-Diethyl 3,3′-[butane-1,4-diylbis(azanediyl]bis(but-2-enoate

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Mohamed Anouar Harrad

2012-10-01

Full Text Available The whole molecule of the title β-enaminoester, C16H28N2O4, is generated by a crystallographic inversion center, situated at the mid-point of the central C—C bond of the 1,4-diaminobutane segment. There are two intramolecular N—H...O hydrogen bonds that generate S(6 ring motifs. This leads to the Z conformation about the C=C bonds [1.3756 (17 Å]. The molecule is S-shaped with the planar central 1,4-diaminobutane segment [maximum deviation for non H-atoms = 0.0058 (13 Å] being inclined to the ethyl butylenonate fragment [C—C—O—C—C=C—C; maximum deviation = 0.0710 (12 Å] by 15.56 (10°. In the crystal, molecules are linked via C—H...O interactions, leading to the formation of an undulating two-dimensional network lying parallel to the bc plane.

4,4-Dimethyl-3,4-dihydropyrido[2′,3′:3,4]pyrazolo[1,5-a][1,3,5]triazin-2-amine ethanol monosolvateFused heterocyclic systems with s-triazine ring. Part 16. for part 15, see Sachdeva et al. (2010.

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Lip Lin Koh

2011-01-01

Full Text Available In the title compound, C10H12N6·C2H5OH, the planarity of the heterocyclic system is slightly distorted at the triazine ring (r.m.s. deviation = 0.1191 Å, which adopts a conformation best described as intermediate between a flattened twisted boat and a half-boat with the tertiary Csp3 atom at the bow. In the crystal, molecules form centrosymmetric dimers connected by N...H—O and O...H—N hydrogen bonds between the amino group H atom, the ethanol solvent molecule and the triazine N atom, making an R44(12 graph-set motif. The other H atom of the amino group and the H atom on the endocyclic N atom form N...H—N hydrogen bonds with the N atoms of the pyrazole and pyridine rings, respectively, linking the molecules into C(7C(7 chains with the R22(8 binary graph-set motif running along [010].

Diethyl 3H-naphtho[2,1-b]pyran-2,3-dicarboxylate

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Abdullah Mohamed Asiri

2009-04-01

Full Text Available The sp3-hybridized methine C atom in the title compound, C19H18O5, lies out of the mean plane of the remaining 13 atoms of the naphthopyran fused-ring system by 0.571 (1 Å, and its H atom occupies a pseudo-equatorial site.

Complete fusion of the 12C+12O, 14N+12C and 15N+12C systems

International Nuclear Information System (INIS)

Conjeaud, M.; Gary, S.; Harar, S.; Wieleczko, J.P.

1978-01-01

Cross sections for evaporation residues following the complete fusion of the 12 C+ 12 C, 14 N+ 12 C and 15 N+ 12 C systems have been measured with a E-ΔE counter telescope in a wide range of incident energies. They are fairly well reproduced by evaporation calculations based on the statistical theory. The total fusion excitation function of the 12 C+ 12 C system shows strong structure, which is compared to the predictions of the reaction cross sections derived from coupled channel calculations and to the integrated inelastic cross sections. Critical angular momenta have been obtained from the fusion cross-section data and these values are discussed in the framework of compound nucleus and entrance channel effects. A striking difference is observed between the fusion cross sections of the 14 N+ 12 C and 15 N+ 12 C systems and shows the importance of the valence nucleons of colliding ions in the fusion process. A possible interpretation might be the influence of the yrast line of the compound nuclei. (Auth.)

1,5-Bis(2-hydroxy-3-methoxybenzylidenecarbonohydrazide methanol 0.47-solvate

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Mouhamadou Moustapha Sow

2014-04-01

Full Text Available In the title compound, C17H18N4O5·0.47CH3OH, the virtually planar (r.m.s. deviation = 0.128 Å carbonohydrazide molecule is located on a twofold axis and conformation of its C=N bonds is E. There are short intramolecular O—H...N hydrogen bonds between the hydroxy groups and hydrazide N atoms. In the crystal, bifurcated N—H...(O,O hydrogen bonds assemble the carbonohydrazide molecules into a three-dimensional network. There are C2 symmetric voids in this network, 47% of which are occupied by disordered methanol molecules.

Synthesis of carbon C-14 labelled 2-phenyl-4-alpha-alkylaminomethyl-quinolinemethanol: a potential anti-leishmaniasis agent

Energy Technology Data Exchange (ETDEWEB)

Wang, T.S.T.; Fawwaz, R.A.; Heertum, R.L.van [Columbia Univ., New York, NY (United States). Coll. of Physicians and Surgeons

1995-07-01

Using sodium acetate, [1-{sup 14}C] as a starting material, a total of seven steps were required to synthesize the title compound. This involved acylation of ortho-dichlorobenzene to form dichloroacetophenone, [2-{sup 14}C] (I). The 2-phenyl-4-quinoline carboxylic acid, [2-{sup 14}C] (II) was prepared by the Pfitzinger reaction from (1) and dichloroisatin. Compound 11 was converted to the acid chloride (III) by reaction with SOCl{sub 2} in benzene. Grignard condensation reaction of (III) yielded 4-quinolylmethylketone, [2-{sup 14}C] (IV) which was then converted to the bromomethylketone (V). Compound V was reacted with NaBH{sub 4} to form the ethylene oxide (VI). Alkylation of the oxide yielded the title compound (VII). The overall radiochemical yield was 10.1% and the specific activity was 3.0 mCi/mmol, with a radiochemical purity of >99.5%. (author).

39 CFR 211.1 - Disposition of former title 39, U.S.C.

Science.gov (United States)

2010-07-01

... 39 Postal Service 1 2010-07-01 2010-07-01 false Disposition of former title 39, U.S.C. 211.1... REGULATIONS § 211.1 Disposition of former title 39, U.S.C. Except as otherwise continued in effect as postal regulations, all provisions of former title 39, U.S.C., which were continued in effect as regulations of the...

Evaluation of radiation dose resulting from the ingestion of [3H]-and [14C]thymidine in the rat

International Nuclear Information System (INIS)

Takeda, H.; Iwakura, T.

1987-01-01

Average doses to rat tissues from the ingestion of 2-[ 14 C]thymidine were compared with those from methyl-[ 3 H]thymidine or 6-[ 3 H]thymidine. [ 14 C]thymidine gave the highest dose to spleen and small intestine. Doses to other tissues from [ 14 ]thymidine were almost the same or lower compared with those from [ 3 H]thymidine, irrespective of the 9 times higher β-ray energy of 14 C than that of 3 H. In the case of [ 14 C]thymidine, most of the dose was given by radioactivity incorporated into the organic tissue constituents (non-volatile radioactivity). In the case of [ 3 H]thymidine, the dose contributions by non-volatile radioactivity were very small and major contributions were rather from volatile radioactivity ( 3 HHO), formed by degradation of [ 3 H]thymidine. No significant difference in their total doses was found between the two [ 3 H]precursors, but the dose from non-volatile radioactivity alone was 2-3 times higher with methyl-[ 3 H]thymidine than with 6-[ 3 H]thymidine. Estimates of dose to cell nuclei in various tissues after ingestion of [ 3 H]thymidine were also made in order to predict more precisely possible radiation hazards. (author)

1-(Prop-2-en-1-yl-3-[(prop-2-en-1-yloxy]quinoxalin-2(1H-one

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Khadija El Bourakadi

2017-05-01

Full Text Available In the title compound, C14H14N2O2, the dihydroquinoxaline moiety deviates slightly from planarity. In the crystal, zigzag chains are formed by inversion-related C—H...O hydrogen bonds. Adjacent chains are associated through pairwise C—H...π(ring and π-stacking interactions.

4-Hydroxy-N′-(4-hydroxy-3-nitrobenzylidenebenzohydrazide

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Zhen Zhang

2011-02-01

Full Text Available The molecule of the title compound, C14H11N3O5, assumes an E configuration with respect to the methylidene unit. An intramolecular O—H...O hydrogen bond is present in the molecule. The dihedral angle between the mean planes of the two benzene rings is 5.46 (15°. The crystal structure is stabilized by intermolecular O—H...O, O—H...N, and N—H...O hydrogen bonds.

Ethyl 2-[(5Z-5-(4-methoxybenzylidene-2,4-dioxo-1,3-thiazolidin-3-yl]acetate

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Hamza Tachallait

2016-07-01

Full Text Available In the title compound, C15H15NO5S, the benzene and heterocyclic rings are close to being coplanar [dihedral angle = 1.49 (6°]. In the crystal, pairwise C—H...O hydrogen bonds form dimers, which are arranged into `stair-step' rows by way of C=O–π interactions between a carbonyl group and the benzene ring [O...π = 3.3837 (12 Å].

Synthesis of the new boron hydride nido-undecaborane(15), B11H15, and the x-ray structure of its conjugate base tetradecahydroundecaborate(1-), [B11H14]-

International Nuclear Information System (INIS)

Getman, T.D.; Krause, J.A.; Shore, S.G.

1988-01-01

The preparation of nido-undecaborane, B 11 H 15 , from the protonation of K[B 11 H 14 ] and the subsequent deprotonation of B 11 H 15 by P(CH 3 ) 3 to give [P(CH 3 ) 3 H][B 11 H 14 ] is described. The structure of [P(CH 3 ) 3 H][B 11 H 14 ] has been determined from single-crystal x-ray data. The spectral data indicate that the boron framework of B 11 H 15 is similar to that of [B 11 H 14 ] - . 11 references, 1 figure

Crystal structure of 2-amino-N-(2-fluorophenyl-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxamide

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K. Chandra Kumar

2015-11-01

Full Text Available In the title compound, C15H15FN2OS, the dihedral angle between the planes of the benzothiophene ring system and the fluorobenzene ring is 3.74 (14°. The six-membered ring of the benzothiophene moiety adopts a half-chair conformation. The molecular conformation is consolidated by intramolecular N—H...F and N—H...O hydrogen bonds. In the crystal, molecules are linked by N—H...O hydrogen bonds, generating C(6 [001] chains.

Labelling by 14C and 3H on 4,4-dimethyl-1-(3,4-methylenedioxyphenyl)-1-pentene-3-ol or stiripentol

International Nuclear Information System (INIS)

Madelmont, J.C.; Rapp, M.; Labarre, P.; Maurizis, J.C.; Dupuy, J.M.; Lepage, F.; Veyre, A.

1992-01-01

4,4-dimethyl-1-(3,4-methylenedioxyphenyl)-1-pentene-3-ol or stiripentol was labelled by 14 C and 3 H. 14 C labelling was performed on the carbon 1 of the pentene group via a four step procedure. The radiochemical yield calculated from the precursor (Ba 14 CO 3 ) is 28%. 3 H labelling was performed on the position 3 of the pentene chain by reduction of the corresponding ketone via NaBT 4 . The radiochemical yield calculated from the precursor (NaBT 4 ) is 40%. (author)

Synthesis of 5-Substituted 3-Amino-1H-Pyrazole-4-Carbonitriles as Precursors for Microwave Assisted Regiospecific Syntheses of Pyrazolo[1,5-a]Pyrimidines

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Fawzia Al-Qalaf

2008-12-01

Full Text Available A simple route to 3-oxoalkanonitrile 5, aprecursor of the title compounds is described. Reaction of enaminones 2 with hydroxylamine hydrochloride in ethanol yielded aldoximes 3 that were converted readily into 5 in basic medium. This method has been successfully applied with a number of substrates and resulted in excellent yields of the products. Reacting 5 with trichloroacetonitrile afforded 3-amino-2-aroyl-4,4,4-trichloro-2-butenenitriles 6 that condensed with hydrazines to yield 3-amino-1H-pyrazole-4-carbonitrilederivatives 8. Substituted pyrazolo[1,5-a]pyridmidines have been prepared with regioselective condensation reactions of 8 with nonsymmetrical dielectrophiles. The structures of compounds obtained were deduced based on 1H-NMR, 1H-15N HMBC- measurements.

Redox-neutral rhodium-catalyzed C-H functionalization of arylamine N-oxides with diazo compounds: primary C(sp(3))-H/C(sp(2))-H activation and oxygen-atom transfer.

Science.gov (United States)

Zhou, Bing; Chen, Zhaoqiang; Yang, Yaxi; Ai, Wen; Tang, Huanyu; Wu, Yunxiang; Zhu, Weiliang; Li, Yuanchao

2015-10-05

An unprecedented rhodium(III)-catalyzed regioselective redox-neutral annulation reaction of 1-naphthylamine N-oxides with diazo compounds was developed to afford various biologically important 1H-benzo[g]indolines. This coupling reaction proceeds under mild reaction conditions and does not require external oxidants. The only by-products are dinitrogen and water. More significantly, this reaction represents the first example of dual functiaonalization of unactivated a primary C(sp(3) )H bond and C(sp(2) )H bond with diazocarbonyl compounds. DFT calculations revealed that an intermediate iminium is most likely involved in the catalytic cycle. Moreover, a rhodium(III)-catalyzed coupling of readily available tertiary aniline N-oxides with α-diazomalonates was also developed under external oxidant-free conditions to access various aminomandelic acid derivatives by an O-atom-transfer reaction. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

10-Ethyl-3-(5-methyl-1,3,4-oxadiazol-2-yl-10H-phenothiazine

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Li-Cheng Sun

2012-03-01

Full Text Available In the title compound, C17H15N3OS, the phenothiazine ring system is slightly bent, with a dihedral angle of 13.68 (7° between the benzene rings. The dihedral angle between the oxadiazole ring and the adjacent benzene ring is 7.72 (7°. In the crystal, a π–π interaction with a centroid–centroid distance of 3.752 (2 Å is observed between the benzene rings of neighbouring molecules.

Synthesis of 1-(2,3-dihydroxypropyl)-2-nitro-1H-imidazole-2-14C and N-(2-hydroxyethyl)-2-(2-nitro-1H-imidazol-1-YL-2-14C)acetamide

International Nuclear Information System (INIS)

Fong, M.T.; Leaffer, M.A.

1986-01-01

We have prepared the 14 C-labeled analogs of NSC 261036, 1-(2,3-dihydroxypropyl)-2-nitro-1H-imidazole-2- 14 C, and NSC 301467, N-(2-hydroxyethyl)-2-(2-nitro-1H-imidazol-1-yl-2- 14 C) acetamide, for pharmacological, drug distribution, and mechanisms of action studies. The latter is an analog designed for lower toxicity and improved properties. The former is a metabolite of, and appears to be less toxic than, misonidazole. (author)

Labelling by [sup 14]C and [sup 3]H on 4,4-dimethyl-1-(3,4-methylenedioxyphenyl)-1-pentene-3-ol or stiripentol. Marquage par [sup 14]C et [sup 3]H du 4,4-dimethyl-1-(methylendioxy-3,4 phenyl)-1-petene-3-ol ou stiripentol

Energy Technology Data Exchange (ETDEWEB)

Madelmont, J.C.; Rapp, M.; Labarre, P.; Maurizis, J.C. (Institut National de la Sante et de la Recherche Medicale (INSERM), 63 - Clermont-Ferrand (France)); Dupuy, J.M. (Centre Jean Perrin, Clermont-Ferrand (France)); Lepage, F. (Laboratoires BIOCODEX, Compiegne (France)); Veyre, A. (Clermont-Ferrand-1 Univ., 63 - Aubiere (France))

1992-11-01

4,4-dimethyl-1-(3,4-methylenedioxyphenyl)-1-pentene-3-ol or stiripentol was labelled by [sup 14]C and [sup 3]H. [sup 14]C labelling was performed on the carbon 1 of the pentene group via a four step procedure. The radiochemical yield calculated from the precursor (Ba[sup 14]CO[sub 3]) is 28%. [sup 3]H labelling was performed on the position 3 of the pentene chain by reduction of the corresponding ketone via NaBT[sub 4]. The radiochemical yield calculated from the precursor (NaBT[sub 4]) is 40%. (author).

Method for combined 3H and 14C autoradiography with a single emulsion tested in cultured mammalian cells

International Nuclear Information System (INIS)

Perdue, S.W.; Kimball, R.F.; Hsie, A.W.

1977-01-01

A single-gelatin expanded film method for double-isotope autoradiography is described. A preliminary classification based upon silver-grain distribution is used to assign labeled cells to 3 H only or with 14 C classes. Optical sectioning combined with grain counting is employed to obtain ratios for classifying cells labeled with 14 C into 14 C only and 3 H + 14 C classes. The method has been tested with CHO-K1 cells in plateau-phase cultures using two 24-h labeling periods. The experimental design allowed for independent estimation of the expected frequencies of label classes under conditions that provided a wide range of possible label levels and combinations. Previous methods have used time-consuming applications of two emulsion layers and exposures to distinguish between cells labeled with 3 H only or with 14 C and do not identify the 3 H + 14 C class. A single-gelatin expanded film requires only one exposure and permits all label classes to be determined by an objective grain-counting procedure

(S-Methyl 2-benzamido-3-(3,4-dimethoxyphenylpropanoate

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Tricia Naicker

2012-01-01

Full Text Available The dimethoxypbenzene ring in the title compound, C19H21NO5, is gauche to the amide group and anti to the ester group. The chirality was confirmed to be S from two-dimensional NMR spectroscopy. In the crystal, N—H...O and C—H...O hydrogen bonds and several short-contact interactions (2.07–3.45 Å create chains parallel to [110]. The phenyl ring is disordered over two orientations in a 0.54 (2:0.46 (2 ratio.

Disposition and metabolism of 14C citrinin in pregnant rats

International Nuclear Information System (INIS)

Reddy, R.V.; Hayes, A.W.; Berndt, W.O.

1982-01-01

Citrinin is a product of fungal metabolism capable of producing nephrotoxicity. Distribution, excretion and metabolism of ( 14 C) citrinin was studied in pregnant female rats after subcutaneous administration of 35 mg/kg on the 12th day of gestation. Elimination of ( 14 C) citrinin-derived radioactivity from plasma was biphasic. The half-lives of the rapid (α) and slower (β) plases of elimination were 1.95 h and 39.7 h, respectively. Approximately 74% of the radioactivity appeared in the urine in the first 24 h, with only 1.7% and 1.4% in the urine at 48 h 72 h, respectively. Fecal elimination accounted for 9.5%, 4.1% and 7.3% of the total radioactivity at each of these times. At least one metabolite of citrinin was demonstrable with high performance liquid chromatography (HPLC) of plasma extracts. Retention times for the parent compound and metabolite were 270 s and 175 s, respectively. The metabolite was more polar than the parent compound. At least 3 metabolites of citrinin were found in urine of the same rats. Retention times for two metabolites were 140 s and 180 s, with both metabolites more polar than the parent compound. Chromatograms of bile samples suggested at least one metabolite was present with a retention time of 140 s. Chromatograms of uterus extracts indicated the presence of one metabolite with a retention time of 180 s. Chromatograms of fetus extracts indicated that no metabolites of citrinin were present. (author)

Crystal structure of 2-bromo-1,4-dihydroxy-9,10-anthraquinone

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Wataru Furukawa

2014-10-01

Full Text Available In an attempt to brominate 1,4-dipropoxy-9,10-anthraquinone, a mixture of products, including the title compound, C14H7BrO4, was obtained. The molecule is essentially planar (r.m.s. deviation = 0.029 Å and two intramolecular O—H...O hydrogen bonds occur. In the crystal, the molecules are linked by weak C—H...O hydrogen bonds, Br...O contacts [3.240 (5 Å], and π–π stacking interactions [shortest centroid–centroid separation = 3.562 (4 Å], generating a three-dimensional network.

Effects of pH upon the environmental fate of [14C]fenitrothion in an aquatic microcosm

International Nuclear Information System (INIS)

Fisher, S.W.

1985-01-01

The environmental fate of [ 14 C]fenitrothion was evaluated in aquatic microcosms held at pH 8.3 or 6.7. No general effect attributable to pH was observed; however, several significant interactions were identified. Of these, the findings that statistically higher amounts of radioactivity were present in water held at pH 6.7 and that significantly less metabolism of the parent compound occurred in the organisms at pH 8.3 were preeminent. These differences seen in metabolism and environmental fate between pH values are relatively minor and do not compromise the safety of the compound

1,3-Bis(4-bromophenylpropane

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Andrew J. Peloquin

2018-04-01

Full Text Available The title compound, C15H14Br2, obtained through the reduction of 4,4′-dibromochalcone, has monoclinic P21 symmetry at 100 K. No directional interactions could be identified in the crystal.

Ethyl 5-cyano-4-[2-(2,4-dichlorophenoxyacetamido]-1-phenyl-1H-pyrrole-3-carboxylate

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Jing Xu

2009-08-01

Full Text Available In the title compound, C22H17Cl2N3O4, the pyrrole ring and the 2,4-dichlorophenyl group form a dihedral angle of 8.14 (13°; the phenyl ring is twisted with respect to the pyrrole ring, forming a dihedral angle of 60.77 (14°. The C=O bond length is 1.213 (3 Å, indicating that the molecule is in the keto form, associated with a –CONH– group, and the amide group adopts the usual trans conformation. The molecule is stabilized by an intramolecular N—H...O hydrogen-bonding interaction. In the crystal, the stacked molecules exhibit intermolecular C—H...O and C—H...N hydrogen-bonding interactions.

3-Chloro-4-methyl­quinolin-2(1H)-one

Science.gov (United States)

Kassem, Mohamed G.; Ghabbour, Hazem A.; Abdel-Aziz, Hatem A.; Fun, Hoong-Kun; Ooi, Chin Wei

2012-01-01

The title compound, C10H8ClNO, is almost planar (r.m.s. deviation for the 13 non-H atoms = 0.023 Å). In the crystal, inversion dimers linked by pairs of N—H⋯O hydrogen bonds generate R 2 2(8) rings. Weak aromatic π–π stacking inter­actions [centroid–centroid distance = 3.7622 (12) Å] also occur. PMID:22589913

Potential antimicrobial agents from triazole-functionalized 2H-benzo[b][1,4]oxazin-3(4H)-ones.

Science.gov (United States)

Bollu, Rajitha; Banu, Saleha; Bantu, Rajashaker; Reddy, A Gopi; Nagarapu, Lingaiah; Sirisha, K; Kumar, C Ganesh; Gunda, Shravan Kumar; Shaik, Kamal

2017-12-01

A series of substituted triazole functionalized 2H-benzo[b][1,4]oxazin-3(4H)-ones were synthesized by employing click chemistry and further characterized based on 1 H NMR, 13 C NMR, IR and mass spectral studies. All the synthesized derivatives were screened for their in vitro antimicrobial activities. Further, molecular docking studies were accomplished to explore the binding interactions between 1,2,3-triazol-4-yl-2H-benzo[b][1,4]oxazin-3(4H)-one and the active site of Staphylococcus aureus (CrtM) dehydrosqualene synthase (PDB ID: 2ZCS). These docking studies revealed that the synthesized derivatives showed high binding energies and strong H-bond interactions with the dehydrosqualene synthase validating the observed antimicrobial activity data. Based on antimicrobial activity and docking studies, the compounds 9c, 9d and 9e were identified as promising antimicrobial leads. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fate of 15N and 14C from labelled plant material

DEFF Research Database (Denmark)

Rasmussen, Jim; Gjettermann, Birgitte; Eriksen, Jørgen

2008-01-01

strength of labelled plant residues in dissolved inorganic N (DIN) and dissolved organic N (DON) in pore water from the plough layer, and (ii) the plant uptake of organically bound N. Litterbags containing 14C- and 15N-labelled ryegrass or clover roots or leaves were inserted into the sward of a ryegrass......–clover mixture in early spring. The fate of the released 14C and 15N was monitored in harvested biomass, roots, soil, and pore water percolating from the plough layer. No evidence of plant uptake of dual-labelled organic compounds from the dual-labelled residues could be observed. N in pore water from the plough...

Synthesis, characterization, electrochemical investigation and antioxidant activities of a new hybrid cyclohexaphosphate: Cu1.5Li(C2H10N2)P6O18·7H2O

Science.gov (United States)

Sleymi, Samira; Lahbib, Karima; Rahmouni, Nihed; Rzaigui, Mohamed; Besbes-Hentati, Salma; Abid, Sonia

2017-09-01

A new organic-inorganic hybrid transition metal phosphate, Cu1.5Li(C2H10N2)P6O18·7H2O, has been prepared and characterized by X-ray diffraction, spectroscopy (infrared, Raman, diffuse reflectance and UV-Vis) and thermal analysis (TG). In addition, its electrochemical behaviors, as well as its antioxidant and antibacterial activities, have been investigated. Its structure is built up by the alternate linkages between copper and phosphate polyhedra, forming puckered layers with intersecting 12-membered rings, in which the ethylenediammonium cations reside. This compound is the first framework structure constructed from cyclohexaphosphates and three distinct copper cations. Cyclic voltammetry study in an acetonitrile solution reveals the facile anodic oxidation of its organic part on a platinum disk and a progressive growing of a thin film, though the repetitive cycling of potential. The title compound was tested for its in vitro antioxidant activities by 1,1-diphenyl-2-picrylhydrazyl (DPPH), 2,2‧-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), Ferrous chelating ability (FIC) and Ferric Reducing Power (FRP) methods. The antioxidant activity of Cu1.5Li(C2H10N2)P6O18·7H2O was analyzed simultaneously with its antibacterial capacity against Escherichia coli, Salmonella typhimurium, Staphylococus aureus, Enterococcus feacium, Streptococcus agalactiae and Candida albicans. The tested compound showed significant antioxidant activities with low antibacterial properties.

Underestimation of glucose turnover measured with [6-3H]- and [6,6-2H]- but not [6-14C]glucose during hyperinsulinemia in humans

International Nuclear Information System (INIS)

McMahon, M.M.; Schwenk, W.F.; Haymond, M.W.; Rizza, R.A.

1989-01-01

Recent studies indicate that hydrogen-labeled glucose tracers underestimate glucose turnover in humans under conditions of high flux. The cause of this underestimation is unknown. To determine whether the error is time-, pool-, model-, or insulin-dependent, glucose turnover was measured simultaneously with [6-3H]-, [6,6-2H2]-, and [6-14C]glucose during a 7-h infusion of either insulin (1 mU.kg-1.min-1) or saline. During the insulin infusion, steady-state glucose turnover measured with both [6-3H]glucose (8.0 +/- 0.5 mg.kg-1.min-1) and [6,6-2H2]glucose (7.6 +/- 0.5 mg.kg-1.min-1) was lower (P less than .01) than either the glucose infusion rate required to maintain euglycemia (9.8 +/- 0.7 mg.kg-1.min-1) or glucose turnover determined with [6-14C]glucose and corrected for Cori cycle activity (9.8 +/- 0.7 mg.kg-1.min-1). Consequently negative glucose production rates (P less than .01) were obtained with either [6-3H]- or [6,6-2H2]- but not [6-14C]glucose. The difference between turnover estimated with [6-3H]glucose and actual glucose disposal (or 14C glucose flux) did not decrease with time and was not dependent on duration of isotope infusion. During saline infusion, estimates of glucose turnover were similar regardless of the glucose tracer used. High-performance liquid chromatography of the radioactive glucose tracer and plasma revealed the presence of a tritiated nonglucose contaminant. Although the contaminant represented only 1.5% of the radioactivity in the [6-3H]glucose infusate, its clearance was 10-fold less (P less than .001) than that of [6-3H]glucose. This resulted in accumulation in plasma, with the contaminant accounting for 16.6 +/- 2.09 and 10.8 +/- 0.9% of what customarily is assumed to be plasma glucose radioactivity during the insulin or saline infusion, respectively (P less than .01)

6-Bromo-1,3-di-2-propynyl-1H-imidazo[4,5-b]pyridin-2(3H-one

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S. Dahmani

2010-04-01

Full Text Available The room-temperature reaction of propargyl bromide and 6-bromo-1,3-dihydroimidazo[4,5-b]pyridin-2-one in dimethylformamide yields the title compound, C12H8BrN3O, which features nitrogen-bound propynyl substituents. The imidazopyridine fused ring is almost planar (r.m.s. deviation = 0.011 Å; the propynyl chains point in opposite directions relative to the fused ring. One acetylenic H atom is hydrogen bonded to the carbonyl O atom of an inversion-related molecule, forming a dimer; adjacent dimers are linked by a second acetylene–pyridine C—H...N interaction, forming a layer motif.

Textural and mechanical characterization of C-S-H gels from hydration of synthetic T1-C3S, β-C2S and their blends

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Dolado, J. S.

2011-06-01

Full Text Available The textural and mechanical characterization of C-S-H gels formed from the hydration of pure T1-C3S, β-C2S and their blends are studied by Nitrogen sorption and nanoindentation experiments. The surface area and nanoporosity of C-S-H gels formed from the hydration of β-C2S and the 30-70 (T1-C3S and β-C2S mixture are higher than those from hydration of T1-C3S, and 70-30, with the difference decreasing with hydration age. Such changes are well supported by findings of nanoindentation study, which shows the greater relative volume of C-S-H phases with lower densities in the β-C2S and the 30-70 pastes. With the increase in hydration age, the relative volume of C-S-H phases with higher densities increased at the expenses of those with lower density. Important quantitative correlations were found among these textural characteristics and the mean chain length, determined from 29Si magic-angle-spinning (MAS NMR, of the C-S-H gels.La caracterización textural y mecánica de geles C-S-H formados a partir de la hidratación de muestras puras de T1-C3S, ß-C2S y sus mezclas ha sido estudiada por medio de adsorción de nitrógeno y nanoindentación. El área superficial y la nano-porosidad de los geles formados durante la hidratación del ß-C2S y la mezcla 30-70 (T1-C3S- ß-C2S son mayores que los correspondientes a los geles del T1-C3S, y la mezcla 70-30; esta diferencia disminuye con el tiempo de hidratación. Estos cambios coinciden con los resultados de nanoindentación que indican un aumento de volumen relativo de las fases C-S-H con una densidad menor en el caso del ß-C2S y la mezcla 30-70. Al aumentar el tiempo de hidratación, el volumen relativo de fases C-S-H de mayor densidad aumenta a expensas de aquellas de menor densidad. Importantes correlaciones cuantitativas se establecen entre las características texturales y la longitud de cadena media del gel C-S-H, determinada mediante RMN-MAS de 29Si.

Microwave assistant synthesis, crystal structure and biological activity of a 1,2,4-triazole compound

International Nuclear Information System (INIS)

Ke, W.; Sun, N.B.

2013-01-01

The title compound (C/sub 17/H/sub 14/F/sub 2/N/sub 4/SO) were synthesized and recrystallized from CH/sub 3/CN. The compound was characterized by 1h-nmr, ftir, ms, hrms and x-ray diffraction. the compound crystallized in the monoclinic space group c2/c with a = 27.532(6), b 8.9596(18), c 14.609(3) alpha = 90, beta = 112.59(3), lambda =90 degree, gamma = 3327.1(12) alpha 3, z = 8 and r = 0.0327 for 2596 observed reflections with 1 > 2 (i). x-ray analysis reveals that not only intermolecular N-H-N interactions, but also C-H Pie stacking interactions exist in the adjacent molecules. The biological activities results showed that it exhibited significant herbicidal activity towards brassica napus. (author)