Crystal Structure and Biological Activities of N-（5-（4-Chloro-2-（trifluoromethyl）phenyl）furan-2-carbonyl）-N＇-（4,6,dimethylpyrimidin-2-yl）thiourea

The new title compound N-（5-（4-chloro-2-（trifluoromethyl）phenyl）furan-2-carbon-yl）- N＇-（4,6-dimethylpyrimidin-2-yl）thiourea （C19H14C1F3N4O2S） has been synthesized, and its crystal structure and biological behaviors were studied. The title compound crystallizes in the monoclinic system, space group P21/c with a = 7.932（5）, b = 33.46（2）, c = 7.556（5） A, β = 98.058（9）°, V = 1986（2） A^3 Mr = 454.85, Z = 4, Dc = 1.521 g/cm^3, μ = 0.349 mm^-1 and F（000） = 928. The structure was solved by direct methods and refined to R = 0.0724 and wR= 0.1429 for 3494 observed reflections （I 〉 2σ（I））. Intermolecular hydrogen bonds along the b axis together with the continuous π-π interactions construct the three-dimensional architecture of the title compound. The preliminary biological tests show definite herbicidalactivity for the title compound.     

Synthesis,Crystal Structure and Biological Activities of N-（4-Cyanopyrazole-3-yl）- α-（3,5-difluorophenyl）- O,O-diisopropyl- α-aminophosphonate

The title compound has been synthesized by the addition reaction of N-（4-cyanopyrazole-3-yl）-3,5-difluorophenyl-imine and diisopropyl phosphate. Its structure was confirmed by means of IR, ^1H NMR and elemental analysis. The single-crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in monoclinic, space group C2/c with a = 18.9959（14）, b = 9.2212（7）, c = 22.1108（16）A^°, β= 90.1540（10）°, V = 3873.0（5） A^°^3, Dc = 1.366 g/cm^3, Z = 8, μ = 0.185, F（000） = 1664, and the final R = 0.0503 and wR = 0.1539 for 2996 observed reflections （I 〉 2σ（I））. The results demonstrate that the dihedral angle between the pyrazole and benzene rings is 105.5°, and there is a full delocalized pyrazole system with sp^2 hydridization of N（3）. The crystal structure is stabilized by two intermolecular hydrogen bonds of N（1）-H（1）…O（3） and N（3）-H（3A）…N（4）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Synthesis and Crystal Structure of （Z）-Ethyl-4-（4-methoxy）benzyndene-2-（3,5- dimethoxypheny-tetrahydrofuran-3,3-dicarboxylate

The title compound （Z）-ethyl-4-（4-methoxy）benzylidene-2-（3,5-dimethoxyphenyl）- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1, with a = 8.140（3）, b = 11.966（4）, c = 13.771（5）Aα= 67.366（4）, β= 85.165（5）, γ= 75.806（4）°, V = 1200.1（7） A3, Z = 2, C26H3008, Mr = 470.50, Dc = 1.302 g/cm^3, F（000） = 500,λ（MoKa） = 0.71073 A, μ= 0.096 mm^-1, R = 0.0659 and wR = 0.1841 for 3080 observed reflections （I 〉 2σ（I））. As a key intermediate of HIV-1 integrase inhibitor, the synthesis and structure confirmation of the title compound are important for further studies.     

Synthesis, Crystal Structure and Antitumor Activity of （E）-4-tert-Butyl-N-（2,4-dichlorobenzylidene）-5-（1,2,4-triazol-1-yl）-thiazol-2-amine

The title compound (E)-4-tert-butyl-N-(2,4-dichlorobenzylidene)-5-(1,2,4-triazol-1-yl)-thiazol-2-amine was synthesized by the reaction of 4-tert-butyl-5-(1,2,4-triazol-1-yl)-thiazol-2-amine with 2,4-dichlorobenzaldehyde, and its crystal structure was determined by singlecrystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.9748(4), b = 10.1803(5), c = 11.4603(6), α = 102.882(1), β = 100.253(1), γ = 104.457(1)°, V = 850.95(7)3, Z = 2, F(000) = 392, C16H15Cl2N5S, Mr = 380.29, Dc = 1.484 g/cm3, S = 1.095, μ = 0.512 mm-1, the final R = 0.0301 and wR = 0.0965 for 3334 observed reflections (I 2σ(I)). The preliminary antitumor activity shows that for the title compound the IC50 of Hela is 0.175 μmol/mL and that of Bel7402 is 0.156 μmol/mL.     

Synthesis and Crystal Structure of 3-（2,4-Dichlorophenyl）- 4-dydroxy-5-cyclohexanyl-△3-dihydrofuran-2-one

The title compound 3-（2,4-dichlorophenyl）-4-dydroxy-3-（2,4-dichlorophenyl）-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-（2,4-dichlorophenyl-acetyl）-1-hydroxycyclo-hexane-carboxylate 4, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.8192（3）, b = 10.5053（5）, c = 10.5811（5）A,α = 71.681（10）, β = 78.905（12）, γ = 81.036（12）°, C15H14C1203, Mr = 313.18, V= 702.44（6）A3, Z = 2, De= 1.481 g/cm^3, F（000） = 324,μ = 0.465 mm^-1, S = 1.006, the final R = 0.0331 and wR = 0.1363 for 2505 observed reflections with I 〉 2σ（I） and 183 variable parameters. The crystal analysis shows that the cyclohexene unit of the title compound has a quasi-chair conformation, and a one-dimensional chain structure is formed via the intermolecular hydrogen bond O（1）-H（101）…O（2）.     

Anti-tumor Metastasis and Crystal Structure of N1（1,3,4-Thiadiazole-2-yl）-N3-m-chlorobenzoyl-urea

The title compound N 1-(1,3,4-thiadiazole-2-yl)-N 3-m-chlorobenzoyl-urea (C 9 H 7 N 4 OSCl,M r=254.70) was prepared by the reaction of m-chlorophenyl isocyanate with 2-amino-1,3,4-thiadiazole in dry acetonitrile.The effect of the title compound on tumor metastasis was analyzed by Lewis-lung-carcinoma model.The bioassay showed that the title compound significantly reduced the number of lung metastasis.The crystal structure has been determined by X-ray diffraction.The crystal belongs to the monoclinic system,space group P2 1 /c with a=11.565(2),b=9.5616(19),c=10.221(2),β=111.75(3)°,Z=4,V=1049.8(4)3,D c=1.612 Mg/m 3,F(000)=520,μ(MoKa)=0.544 mm-1,R=0.0468 and wR=0.0922 for 1236 observed reflections (I > 2σ(I)).     

Synthesis,Crystal Structure and Fungicidal Activity of （E）-2-[（4-tert-Butyl-5-（4-methoxybenzyl）thlazol-2 yhmino）methyl]phenol

The title compound （E）-2-[（4-tert-butyl-5-（4-methoxybenzyl）thiazol-2-ylimino）methyl]phenol was synthesized by the reaction of 5-（4-methoxybenzyl）-4-tert- butylthiazol-2-amine with salicylaldehyde, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 5.9362（8）, b = 11.5070（15）, c = 29.460（4）A, β= 97.326（3）°, V = 1995.9（5） A^3, Z = 4, F（000） = 808, C22H24N2O2S, Mr= 380.49, De= 1.266 g/cm^3, S = 1.031,μ = 0.181 mm^-1, the final R = 0.0474 and wR = 0.1441 for 4327 observed reflections （I 〉 2σ（I））. Intramolecular O-H…N hydrogen bond is observed in the crystal. The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.     

Synthesis,Crystal Structure and Biological Activity of 1-（β-D-Glucopyranosyl）-3- amino-5-methyl-1H-1,2,4-triazole

The title compound 1-（β-D-glucopyranosyl）-3-amino-5-methyl- 1H- 1,2,4-triazole was synthesized and characterized by IR, 1H-NMR and elemental analysis. Its single crystals of 2H2O adduct suitable for X-ray analysis were obtained by the slow evaporation of a H2O solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 7.7490（15）, b = 10.424（2）, c = 17.447（4） A^°, V = 1409.3（5） A^°^3, Z= 4, C9H20N4O7, Mr = 296.29, Dc = 1.396 g/cm^3,μ = 0.120 mm^-1, S = 1.007, F（000） = 632, R = 0.0686 and wR = 0.1560 for 1217 observed reflections with I 〉 20（I）. The title molecules are linked through intermolecular hydrogen bonds to form two 1-D chain structures, and such adjacent chains are further linked by intermolecular hydrogen bonds and H2O bridges to form a 3-D supramolecular network structure. The preliminary bioassay results showed that the title compound exhibits fungicidal activities against Gibberella zeae and Colletotrichum orbiculare.     

Synthesis and Crystal Structure of （Z）-5-fluoro-3- （phenyl（（5-（pyridin-3-ylmethyl）thiophen-2- yl）amino）methylene） Indolin-2-one

The crystal structure of the title compound （Z）-5-fluoro-3-（phenyl（（5-（pyridin-3- ylmethyl）thiophen-2-yl）amino）methylene） indolin-2-one （C25H18FN3OS, Mr = 427.50） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 5.931（1）, b = 12.413（1）, c = 28.102（2） A, V= 2090.4（3） A3, Z = 4, Dc = 1.358 g/cm3, F（000） = 888, μ= 0.186 mm-1, MoKa radiation （2 = 0.71073）, R = 0.041 and wR = 0.105 for 4567 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the indole and thiophene rings are not coplanar with a dihedral angle of 46.26（5）°. Intramolecular and intermolecular N-H＇..O hydrogen bonds together with C-H...π interations can be observed in the lattice.     

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 1-（Trifluoromethyl）-1-（propioloyl）-（E）-3-oxo-（2-thienyl）-（2-naphthylamine）

1INTRODUCTIONTheSchiffbasesderivedfromb-diketonesandaliphaticamineshavebeenshowntoexistastheketo-amines.However,ifsubstituentseitherattheketooraminogrouparearomatic,itmaybeexpectedtheenoliminewillbethefavoredtautomericform[1].Recently,someSchiffbasesderivedfromTTA(4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione)andPMBPhavebeenstudiedbyWang[2]andYu[3]etal.Inordertostudytherelationshipbetweenthestructuresandperformancesofthesecompounds,thetitlecom-poundwillbereportedherein.2EXPERIMENT…     

Synthesis and Crystal Structure of 1-[4-(Pyrimidin-2-yl)piperazin-1-ylmethyl]-1H-benzotriazole

1 INTRODUCTION Based on the reported 1.65 ? high resolution crystal structure of spinach KARI (ketol-acid reduc- toisomerase) complex[1], we obtained 279 molecules with low binding energy toward KARI from MDL/ ACD 3D database searching, using program DOCK 4.0[2]. These potential structures provide further information for the design of new KARI inhibitors, one of novel derivatives of which as the title com- pound has been synthesized. Its crystal structure will provide us more inf…     

Synthesis and Crystal Structure of （S）-Ethyl-2-（2-methoxy-phenylsulfenamido）-3-（1H-indol-3-yl）propanoate

With an aim to discover novel AHAS inhibitors,the title compound (S)-ethyl-2(2-methoxy-phenylsulfenamido)-3-(1H-indol-3-yl)propanoate (C 21 H 22 N 2 O 4 S,M r=398.47) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis.The crystal belongs to orthorhombic,space group P2 1 2 1 2 1 with a=8.078(2),b=12.824(4),c=18.788(6),V=1946.2(10) 3,Z=4,F(000)=840,D c=1.360 mg/m 3,μ=0.197 mm-1,the final R=0.0433 and wR=0.1035 for 3075 observed reflections with I > 2σ(Ⅰ).The absolute structure Flack parameter X of this compound is 0.00(8).A total of 14375 reflections were collected,of which 3431 were independent (R int=0.0437).X-ray analysis reveals that the crystal structure involves two intermolecular N-H···O and one N-H···S intermolecular hydrogen bonds with the neighboring molecules.The crystal structure was compared with our previously reported (S)-methyl 2-(4-R-phenylsulfonamido)-3-(1H-indol-3-yl)propanoate (R=H(1) and Cl(2)),which provided some useful information of these compounds.     

Chiral Phosphine Ligands Derived from Sugars 4.Crystal Structure of Methyl 4,6-O-Benzylidene-3-Deoxy-3-(Diphenylphosphino)-α-D-Altropyranoside (3-MBPA)

IINTRODUCTIONChiralphosphinesareveryusefulligandsinenantioselectivecatalysiswithtransitionmetalcomplexes"'.Becausesugarisrichnotonlyinstereochemistrybutalsoinnatureandpossessesmanyhydroxylgroupsassyntheticstartingpoints,theyhavereceivedmuchattentionsincethe1970st2i.However,thetypesofchiralphosphinesinwhichthephosphorusatomsareattacheddirectlytothesecondarycarbonsofsugararefew.Thedifficultiesinthesyntheticprocessesarepartofthereason.Bythenucleophilicreplacementreaction,itisdifficulttolink…     

Synthesis and Crystal Structure of 4-(2-Methylene-1-ethyl-3,3-dimethylindoline-2'-yl)-6,8-dibromo- 1'-ethyl-3',3'-dimethylspiro-[3,4-dihydro-2H-1-benzopyran-2,2'-indoline]

The title compound of 4-(2-methylene-1-ethyl-3,3-dimethylindoline-2'-yl)-6,8-dibro-mo-1'- ethyl-3',3'-dimethylspiro[3,4-dihydro-2H-1-benzopyran-2,2'-indoline],C33H36Br2N2O,as a dicondensed spiropyran (DC) has been synthesized by indoline in ethanol with 3,5-dibromo-salicyaldehyde.The compound was characterized by elemental analysis and IR spectra.Meanwhile,the crystal of the compound was obtained and determined by X-ray single-crystal diffraction.Crystal data: monoclinic system,space group P21/n,a=12.9699(15),b=12.5196(13),c=19.327(2) (A),β=106.493(3)°,Mr=636.46,V= 3009.1(6) (A)3,Z=4,F(000)=1304,Dc=1.405 g/cm3,μ=2.722 mm-1,R=0.0554 and wR=0.1176 for 6892 independent reflections (Rint=0.0354) and 5699 observed reflections (I>2σ(I)).     

Synthesis and Crystal Structure of 2-Amino-4- chloro-5-（4-methylbenzyl）-6-methylpyrimidine

The title compound 2-amino-4-chloro-5-(4-methylbenzyl)-6-methylpyrimidine (C26H28Cl2N6, Mr = 495.44) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 14.892(7), b = 6.129(3), c = 14.889(7) , β = 109.795(8)°, V = 1278.7(10) 3, Z = 2, F(000) = 520, Dc = 1.287 g/cm3, μ = 0.280 mm-1, the final R = 0.0577 and wR = 0.1589 for 1357 observed reflections with I > 2σ(I). A total of 6091 reflections were collected, of which 2257 were independent (Rint = 0.033). The X-ray analysis reveals that the chlorine atom and methyl of the title compound are disordered.     

Synthesis and Crystal Structure of（E）-Ethyl 2-（4-（2,4-dimethoxybenzylideneamino）-5-（3,4,5-trimethoxyphenyl）-4H-1,2,4-triazol-3-ylthio）acetate

The crystal structure of the title compound(E)-ethyl 2-(4-(2,4-dimethoxy benzylide-neamino)-5-(3,4,5-trimethoxyphenyl)-4H-1,2,4-triazol-3-ylthio)acetate(4,C24H28N4O7S,Mr = 516.17) was synthesized and determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 13.162(2),b = 8.4506(13),c = 22.602(4) ,β = 99.888(3)°,μ = 0.183 mm-1,V = 2476.5(7)3,Z = 4,Dc = 1.385 g/cm3,F(000) =1088,T = 110(2) K,R = 0.0426 and wR = 0.1216 for 3859 observed reflections with I > 2σ(Ⅰ).     

Synthesis and Crystal Structure of (Z)-4-(p-Bromo phenylthio)-3-(p-nitrobenzoyloxy)-3-buten-2-one

１　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｏｒｄｅｒｔｏｅｖａｌｕａｔｅｔｈｅｓｅｌｅｃｔｉｖｉｔｙａｎｄｒｅａｃｔｉｖｉｔｙｏｆｅｎｏｎｅｓａｓｄｉｅｎｏｎｅｐｈｉｌｅｓａｎｄｄｉｅｎｅｓｉｎＤｉｅｌｓＡｌｄｅｒｒｅａｃｔｉｏｎ,Ｐａｒａｌｔａｓｙｎｔｈｅｓｉｚｅｄβｆｕｎｃｔｉｏｎａｌｉｚｅｄｌａｃｅｔｙｌｖｉｎｙｌａｒｅｎｅｃａｒｂｏｘｙｌａｔｅｓａｓａｓｕｂｓｔｒａｔｅｏｆ１,３ｄｉｐｏｌａｒｃｙｃｌｏａｄｄｉｏｎｒｅａｃｔｉｏｎ〔１〕．Ｘｒａｙｃｒｙｓｔａｌｌｏｇｒａｐｈｉｃｓｔｕｄ…     

Crystal Structure of 3-Methyl-4-methoxy-3-(3-methyl-4- methoxy-2-benzofuranyl) -2-H-benzofuranyl

1　ＩＮＴＲＯＤＵＣＴＩＯＮ3ｍｅｔｈｙｌ4ｈｙｄｒｏｘｙｂｅｎｚｏｆｕｒａｎｉｓａｎｉｎｔｅｒｍｅｄｉａｔｅｕｓｅｄｆｏｒｔｈｅｓｙｎｔｈｅｓｉｓｏｆｎａｔｕｒｅｐｒｏｄｕｃｔｓ[1].Ｉｔｈａｓｂｅｅｎｓｙｎｔｈｅｓｉｚｅｄｆｒｏｍ1,3ｄｉｈｙｄｒｏｘｙｂｅｎｚｅｎｅ[2-3].Ｔｏｓｙｎｔｈｅｓｉｚｅａｂｉｅｔａｎｅｑｕｉｎｏｎｅｄｉｔｅｒｐｅｎｏｉｄｓｗｉｔｈｉｔ[4,5],ｗｅｉｎｔｅｎｄｅｄｔｏｐｒｏｔｅｃｔｔｈｅｈｙｄｒｏｘｙａｔｔａｃｈｅｄｔｏｉｔｗｉｔｈＭｅ2ＳＯ4.Ｆｉｎａｌｌｙ,ｔｗｏｃｏｍｐｏｕ…