Synthesis and Crystal Structure of 2,3,4,6-tetra-O-Acetyl-1-{4-chloro-3-[1-（4-ethoxyphenyl）-1-methylethyl]phenyl}-1-deoxy-β-D-glucopyranose

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system(C31H37ClO10,Mr = 605.06),space group P21 with a = 11.882(5),b = 10.106(5),c = 13.816(6),V = 1545.9(12)3,Z = 2,Dc = 1.300 g/cm3,F(000) = 640,μ = 0.179 mm-1,the final R = 0.0430 and wR = 0.0595 for 4960 observed reflections(I > 2σ(I)).The title compound was confirmed to be a β-anomer by single-crystal X-ray diffraction and 1H NMR.The proximal benzene ring is nearly orthogonal to the glucopyranoside ring,and the two benzene rings are also almost orthogonal to each other.Four non-classical intermolecular hydrogen bonds observed in the crystal lattice help to stabilize the crystal.     

Synthesis,Crystal Structure and Biological Evaluation of 4-Chloro-2-(morpholine-4-carbonyl)phenyl-4′-methoxybenzoate as Molluscicidal Agent

The title compound 4-chloro-2-(morpholine-4-carbonyl)phenyl-4'-methoxybenzoate(C19H18ClNO5, Mr = 375.79), a 5-chlorosalicylic acid derivative incorporating morpholine moiety, was conveniently synthesized through two steps and crystallized in the monoclinic space group P21/c with a = 7.8501(10), b = 9.3149(12), c = 25.133(3), V = 1836.2(4)3, Z = 4, Dc = 1.359 Mg/m3, λ = 0.71073, μ(MoKα) = 0.237 mm-1, F(000) = 784, R = 0.0447 and wR = 0.1227 for 3982 independent reflections with I 2σ(I). The dihedral angles formed between 4-methoxybenzene and 5-chlorobenzene rings, the 5-chlorobenzene and morpholine, and 4-methoxybenzene and morpholine rings are 82.55(3), 72.56(5) and 47.68(0)° by X-ray analysis, respectively. Bioassay shows that the title compound has a good molluscidal effect.     

Synthesis,Crystal Structure and Antitumor Activity of N-（4-tert-butyl-5-（4-chlorobenzyl）thiazol-2-yl）-2,6-difluorobenzamide

The title compound was synthesized by the reaction of 4-tert-butyl-5-(4-chlorobenzyl)-2-aminothiazole with 2,6-difluorobenzoic acid. The crystal structure of the title compound, C21H19ClF2N2OS, was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pbca with a = 12.6479(13), b = 13.1204(13), c = 14.1341(15), Z = 4, V = 2011.5(4)3, Mr = 420.89, Dc = 1.390 g/cm3, S = 1.023, μ = 0.326 mm-1, F(000) = 872, the final R = 0.0365 and wR = 0.0880 for 6101 observed reflections(I 2σ(I)), and R = 0.0507, wR = 0.0978 for 7779 independent reflections. X-ray crystal structure displays that the hydrogen bonding interactions observed link the molecules to form a dimeric unit. The preliminary biological test of the title compound shows good antitumor activity, with IC50 of 0.046 μmol/mL against the Hela cell line.     

Synthesis and Crystal Structure of a Luminescent Compound 5-（1H-benzoimidazol-2-yl）- 3H-[ 1,2,3 ] triazole-4-carboxylic Acid

The title compound, 5-(1H-benzoimidazol-2-yl)-3H-[1,2,3]triazole-4-carboxylic acid (C10H7N5O2·C3H7NO, Mr=302.30), has been synthesized and characterized by FT-IR and ESI-MS, 1 H-NMR spectroscopy and X-ray single-crystal diffraction. Crystal structure of the title compound was grown from DMF by slow diffusion at room temperature. Crystal data: orthorhombic structure, space group Pna21 with a=6.9635(3), b=19.4398(7), c=30.6165(12), V=4144.5(3)3, Z=12, Dc=1.454 g/cm 3, μ(MoKα)=0.108 mm-1, and F(000)=1896. The structure was refined to R=0.0450 and wR=0.0975 for 3578 observed reflections with I>2σ(I). The intermolecular hydrogen bonds and π-π stacking further stabilize the structure.     

Preparation and Crystal Structure of 12β,15α-dihydroxyprogesterone

Progesterone(1) was biotransformed into the title compound 12β,15α-dihydroxy-progesterone(2) with Colletotrichum lini AS3.4486.The biotransformation process was monitored with HPLC.The structure of 2 was determined by 1H NMR,13C NMR,ESI-MS and single-crystal X-ray diffraction.The crystal of the compound belongs to orthorhombic,space group P212121 with a = 8.0671(9),b = 12.3970(15),c = 18.532(3) ,Z = 4,V = 1853.3(4)3,Dc = 1.242 mg/m3,μ = 0.084 mm-1,F(000) = 752,R = 0.0373 and wR = 0.0850.Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 2 has been constructed by multiply intermolecular O(2)-H(2)…O(4) and O(3)-H(3)…O(2) H-bonding interactions.     

Synthesis and Characterization of （4R,5R）-1,3-dioxolance-4,5-bis（2-pyridineacrboxylic acid）

The title compound, (4R,5R)-1,3-dioxolance-4,5-bis(2-pyridineacrboxylic acid), has been synthesized and characterized by single-crystal X-ray diffraction, IR, NMR, and MS analyses. Crystal structure of the title compound was grown from ETOH by slow diffusion at room temperature. The title compound crystallizes in monoclinic, space group C2 with a = 17.805(3), b = 11.459(3), c = 11.1656(17) , β = 113.066(4)°, V = 2095.9(6) 3, Z = 4, F(000) = 880, Dc = 1.332 Mg/m-3, C23H20N2O6, Mr = 420.41 and μ = 0.10 mm-1     

Synthesis and Crystal Structure of 3,5-Dichloro-N-(2-methoxyphenyl)benzamide

<正>The title compound was synthesized by the direct reaction of 3,5-dichlorobenzoic acid with 2-methoxyaniline in the presence of DCC and HOBT. The structure was supported by the spectroscopic data and unambiguously confirmed by the single-crystal X-ray diffraction studies. It crystallizes from a methanol solution in the monoclinic space group P2_1/c with unit cell dimensions of a = 4.9369(16), b = 13.351(5), c = 20.168(7), β = 96.755(8)°, V = 1320.1(8)~3 and Z = 4.     

Synthesis, Crystal Structure and Biological Activity of a New 1,2,4-Triazole Derivative

A new 1,2,4-triazole containing cyclopropane moiety was synthesized and characte- rized by 1H NMR, MS and elemental analyses. The crystal structure of the title compound (C13H14FN3S, Mr = 263.33) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 12.614(3), b = 7.0202(14), c = 15.556(3), β = 110.92(3)°, V = 1286.7(4)3 , Z = 4, F(000) = 552, Dc = 1.359 g/cm 3 , μ = 0.25 mm-1 , the final R = 0.0336 and wR = 0.0898 for 2568 observed reflections with Ⅰ > 2σ(Ⅰ). A total of 10093 reflections were collected, of which 3045 were independent (Rint = 0.0268). The herbicidal activity of the title compound was determined, and this compound displays excellent herbicidal activity against Brassica campestris.     

Crystal Structure and Molecular Docking of a Novel 4-(2-Acetonyl-selanyl-benzamido) Benzoic Acid as a Potential Anti-ischemic Stroke Candidate

The title compound 4-(2-acetonyl-selanyl-benzamido) benzoic acid was synthesized and its structure was determined by NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P2_(1/n), with a = 5.18537(19), b = 18.9308(7), c = 16.6586(5) ?, b = 95.857(3)°, V = 1626.72(10) ?~3, Z = 4, D_c = 1.536 g/cm~3, m = 3.302 mm~(-1), F(000) = 760, the final R = 0.0466 and wR = 0.1353 for 2308 observed reflections with I 2σ(I). In silico docking studies were carried out to evaluate the anti-ischemic stroke activities for twenty-one ischemic stroke associated proteins by Autodock 4.2 software. The title compound has better activity against ischemic stroke than Ebselen.     

Synthesis and Crystal Structure of（2E,6E）-2,6-bis（2,3-dimethoxybenzylidene）cyclohexanone

The new title compound (2E,6E)-2,6-bis(2,3-dimethoxybenzylidene)cyclohexanone (C 24 H 26 O 5,M r=394.45) has been synthesized,and its crystal structure was studied.The title compound crystallizes in the orthorhombic system,space group Pca2 1 with a=17.536(2),b=14.8515(16),c=8.0512(9),V=2096.8(4) 3,Z=4,D c=1.250 g/cm 3,λ=0.71073,μ=0.087 mm-1 and F(000)=840.The structure was solved by direct methods and refined to R=0.0533 and wR=0.1248 from 2727 observed reflections (I > 2σ(Ⅰ)).The title molecules are connected through hydrogen bonds to generate a 3-D supramolecule.The preliminary biological tests showed definitely biological activity for the title compound.     

Facile Synthesis and Crystal Structure of a Novel Cyanopyridine

The title compound 2-amino-4-(4-hydroxy-3,5-dimethoxyphenyl)-5-methyl-6-phenyl nicotinonitrile,C 21 H 19 N 3 O 3,was synthesized via four-component reactions between propio-phenone,malononitrile,syringaldehyde and ammonium acetate in ethanol under reflux without catalyst and characterized by IR,1 H NMR,13 C NMR,MS,EA and single-crystal X-ray diffraction.Single-crystal X-ray diffraction analysis shows that the compound is of monoclinic system,space group P2 1 /n with a=8.4600(17),b=17.139(3),c=13.408(3),β=107.06(3)°,V=1858.6(6)3,Z=4,M r=361.39,F(000)=760,μ(MoKα)=0.088 mm-1,D c=1.292 g/cm 3,λ=0.71073,the final R=0.0751 and wR=0.0938 for 3333 observed reflections with I > 2σ(I).The crystal packing of the title compound is stabilized by intermolecular hydrogen bonds.     

Synthesis and Crystal Structure of（S）-N-（hexahydro-2-oxo-1H-azepin-3-yl）-3-phenyl-2-propenamide

The title compound(S)-N-(hexahydro-2-oxo-1H-azepin-3-yl)-3-phenyl-2-propenamide(C15H18N2O2, Mr = 258.31) was synthesized by the reaction of(S)-α-amino-ε-caprolactam with 3-phenyl-2- propenoyl chloride. Its chemical structure was determined by 1H NMR, 13C NMR, H RMS and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/n with a = 14.957(3), b = 4.884(1), c = 18.630(4), β = 95.91(3)o, V = 1353.7(5)3, Z = 4, Dc = 1.267 g/cm3, μ = 0.085 mm-1, F(000) = 552, R = 0.0671 and wR = 0.1547 for 2473 observed reflections with I 2σ(I).     

Crystal Structure and Conformation of an Imino Sugar

The title compound 3 was synthesized and characterized by IR,NMR and H-RMS,and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic system (C16H23NO7S,Mr=373.41),space group P21,with a=12.000(2),b=5.5970(11),c=13.689(3),β=93.25(3)°,V=917.9(3)3,Z=2,Dc=1.351 g/cm3,F(000)=396,μ=0.213 mm-1,the final R=0.0489 and wR=0.0777 for observed reflections (I > 2σ(I)). Three intramolecular and three intermolecular hydrogen bonds were found. The absolute configuration of this molecule was confirmed by comparing with the original material.     

Crystal Structure of Phenol,2-[4（S）-4-Dihydro-4-benzyl-2-ozazolinyl]

The compound phenol,2-[4(S)-4,5-dihydro-4-phenyl-2-ozazolinyl(1,C15H13NO2) was synthesized with a simple,one step method free of water and air.It was obtained in a moderate yield from the reaction of 2-hydroxybenzonitrile with optically active amino alcohol in chloroben-zene under dry,anaerobic conditions.It belongs to the orthorhombic system,space group P212121 with a = 5.786(5),b = 10.730(5),c = 19.722(5),C15H13NO2,Mr = 239.26,V = 1224.4(12)3,Z = 4 and Dc = 1.298 mg/m3.The final R = 0.0324 for 1627 observed reflections with Ⅰ 2σ(Ⅰ) and Rw = 0.0826 for all data.The structure of compound 1 was determined by X-ray diffraction,NMR and HRMS.     

Syntheses,Crystal Structures and Antibacterial Activities of Two New Methyl 12-Alkylamino-13,14-dinitrodeisopropyl-dehydroabietates

The title compounds(5 a and 5 b) were synthesized from dehydroabietic acid and characterized by MS, IR, NMR and elemental analysis. The crystal structure of compound 5 a was determined by single-crystal X-ray diffraction. The compound is of monoclinic system, space group P21 with a = 8.0860(16), b = 14.011(3), c = 9.799(2) ?, β = 106.31(3)?, Z = 2, V = 1065.5(4) ?3, Mr = 431.48, Dc = 1.345 Mg/m3, S = 1.002, μ = 0.099 mm-1, F(000) = 460, the final R = 0.0617 and wR = 0.1532 for 1397 observed reflections(I 2σ(I)). The preliminary antibacterial assay showed that compound 5 a exhibited considerable inhibitory activity against Bacillus subtilis, Staphylococcus aureus and Methicillin-resistant S. aureus(MRSA) with MIC values of 2～8 μg/mL.     

Synthesis,Structure and Biological Activity of 5-Benzyl-4-amino-1,2,4- triazole-3-thione Schiff Base

A novel Schiff base was synthesized via 5-benzyl-4-amino-1,2,4-triazole-3-thione with 3-phenoxy-benzaldehyde under refluxing. The structure was characterized by elemental analysis, IR, 1H NMR, ESI-MS and single-crystal X-ray diffraction. This compound crystallizes in monoclinic, space group P21 /c with a = 16.0289(16), b = 5.8022(6), c = 20.542(2), β = 95.667(2)o, C22 H18 N4 OS, Mr = 386.46, V = 1901.1(3)3, Z = 4, Dc = 1.347 g/cm3, F(000) = 804, μ = 0.191 mm-1, the final R = 0.0453 and wR = 0.1307 for 2456 observed reflections with I 2σ(I). The crystal packing of the compound is stabilized by classical intermolecular N–H···S hydrogen bonds. Furthermore, the biological activity to four vegetable pathogens has been tested. The title compound exhibited good fungicidal activities to Gibberlla nicotiancola.     

Synthesis,Crystal Structure and Biological Activity of N-tert-butyl-N-(4-methyl-1,2,3-thiadiazole)-5-yl-N’-(4-methyl-1,2,3-thiadiazole)-5-formyl-N’-3,5-dichloropyridin-2-yl-diacylhydrazine

The title compound N-tert-butyl-N-(4-methyl-1,2,3-thiadiazole)-5-yl-N'-(4-me-thyl-1,2,3-thiadiazole)-5-formyl-N'-3,5-dichloropyrid-2-yl-diacylhydrazines (C18H17Cl2N7O3S2, Mr = 514.41) has been synthesized by the reaction of N-tert-butyl-N'-3,6-dichloropyridine-2-formyl hydrazine with 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride and triethylamine, and its structure was characterized by 1H NMR, HR MS, and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group C2/c with a = 27.726(8), b = 11.045(3), c = 14.507(4), β = 96.758(4)°, Z = 8, V = 4412(2) 3, Dc = 1.549 g/cm3, μ = 0.521 mm-1, F(000) = 2112, R = 0.0405 and wR = 0.1153. X-ray analysis indicates that all rings are non-planar in this molecule. The bioassay results indicate that both the title compound and the positive control RH-5992 have weak fungicide activities, while the title compound has good insecticidal activity against Plutella xylostella L. and no insecticidal activity against Culex pipiens pallens.     

Synthesis and Crystal Structure of 3-Methyl-10-(4-nitrophenyl)-7,8,10,10a-tetrahydropyrano[4,3-b]chromene-1,9(4aH,6H)-dione

The title compound (C19H15NO6) was synthesized via a three-component reaction and characterized by means of IR and 1H NMR. Its crystal and molecular structures were determined by X-ray diffractometry. It belongs to the monoclinic system, space group P21/c with a = 11.670(3), b = 12.076(3), c = 11.613(3), β = 99.490(4)°, V = 1614.2(7)3, Mr = 353.32, Z = 4, Dc = 1.454 g/cm3, λ = 0.71073, μ = 0.110 mm-1, F(000) = 736, the final R = 0.0503 and wR = 0.1311. A total of 8454 reflections were collected, of which 3497 were independent (Rint = 0.0333) and 2102 were observed with I > 2σ(I).     

Synthesis and Structure Analysis of N-（Dehydroabietyl）maleamic Acid

N-(Dehydroabietyl)maleamic acid was synthesized from dehydroabietylamine and maleic anhydride.Its structure was characterized by IR,1 H-and 13 C-NMR spectra.The stereo structure of the title compound was also unambiguously confirmed by X-ray crystal structure analysis.The white crystal crystallizes in the monoclinic system,space group P2 1 with a=12.075(2),b=10.377(2),c=17.840(4),β=100.31(3) °,V=2199.3(8) 3,R=0.0618 and wR=0.1437.Two crystallographically independent molecules with different conformations co-exist in the unit.In each molecule,the two cyclohexane rings form a trans ring junction with chair and half-chair conformations,respectively.The C=C double bond between two carbonyl groups is in a Z configuration.Intermolecular and intramolecular hydrogen bonds coexist to stabilize the structure.     

Synthesis,Structure and Fluorescence Study of 3-Bromo-7-methyloxy-4-methylcoumarin

Coumarin derivative 3-bromo-7-methyloxy-4-methylcoumarin(C11H9BrO3) was synthesized and characterized by FT-IR,1H NMR spectra,and thermal analysis.The crystal structure was determined by X-ray single-crystal diffraction.The title compound crystallizes in the mono-clinic system,space group P21/n,with a = 7.770(16),b = 12.501(3),c = 10.627(2),β = 98.46(3)°,Mr = 269.09,V = 1021.0(4) 3,Z = 4,Dc = 1.751 g/cm3,μ = 4.008 mm-1,F(000) = 536,R = 0.0650 and wR = 0.1463.The optimization of the title compound was obtained by quantum chemical method at the SVWN5/6-31G** level.In the structure,the measured angles of the crystal structure are similar to those calculated,while the measured bond lengths are shorter than the calculated values due to the crystal field which functions to the molecule.The title compound also shows good fluorescent behaviors and good linear relationship with the equal concentration gradient in methanol.