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）.     

Synthesis,Structure Analysis,and Antitumor Activity of （R）-2,4-Dioxo-5-fluoro-l-[1-（methoxycarbonyl） Ethylaminocarbonylmethyl]-1,2,3,4-tetrahydropyrimidine

A new dipeptide compound, （R）-2,4-dioxo-5-fluoro-1-[1-（methoxycarbonyl） ethylaminocarbonylmethyl]-1,2,3, 4-tetrahydropyrimidine （5-FUAPM）, has been synthesized and identified by means of elemental analysis, IR, ^1H NMR and ^13C NMR spectra. The single crystal of compound 5-FUAPMoDMF was also obtained and characterized by DSC-TGA techniques. The crystal belongs to orthorhombic space group P212121 with the cell parameters： a= 0.4740（7） nm, b= 1.923（3） nm, c= 1.9229 nm, a=β=y=90°, V= 1.753 nm^3, Z=4, Dc= 1.312 g/cm^3, Mr=346.32, F（000）=728 and u=0.111 mm^-1. The final R and wR are 0.1378 and 0.2862, respectively. The result of the biological test showed that the compound 5-FUAPM has certain antitumor activities.     

Synthesis,Crystal Structure and Biological Activity of a Novel Complex： Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-Triazole-yl）-6-chloro-pyridazine）

The title compound, Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-triazole-yl）-6-chloro-pyridazine） 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the triclinic system, space group P1 with a = 6.018（3）, b = 9.832（5）, c = 9.921（5）A, a = 78.270（8）, β = 74.550（8）, γ = 83.807（8）°, V = 553.1（5）A^3, Z = 1, C14H16Cl4CoN10O2, Mr = 557.10, Dc = 1.673 g/cm^3, F（000） = 281,μ（MoKα） = 1.293 mm^-1, the final R = 0.0453 and wR = 0.1181 for 1539 observed reflections with I 〉 2σ（I）. The Co（II） ion is in a distorted centrosymmetric six-coordinate octahedral environment with two Ntriazole, two Omethanol and two Cl atoms. Via hydrogen bonds the configuration of 1 has been extended into 1D chains which are developed to 2D layers via π-π sticking action, and these layers are further extended into a 3D network by hydrogen bonds. The antibacterial activity of the title compound has been detected, and the results show that the ligands and cobalt（II） complex exhibit certain fungicidal activity against several bacteria. Furthermore, the spectral properties of the title compound have been also studied and discussed.     

Synthesis and Crystal Structure of 2-（4-Fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H- 1,2,4-triazol-1-ylmethyl）-3-methoxy-isopropy Alcohol

The title compound 2-（4-fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H-1,2,4-triazol- 1-ylmethyl）-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-（4-fluoro- 2-（4-fluorophenoxy）phenyl）-2,3-epoxypropyl]-1H-1,2,4-triazole with sodium methoxide. It belongs to orthorhombic, space group P212121, with a = 9.7229（19）, b = 11.516（2）, c = 16.047（3）A, C18H17F2 N3O3, Mr = 361.35, V = 1796.7（6）A^3, Z = 4, Dc = 1.3359 g/cm^3, F（000） = 752, p = 0.106 mm^-1, the final R = 0.0329 and wR = 0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56（3） and 54.78（2）°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.     

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,Crystal Structure and Antifungal Activity of N-（Pyridine-2-methyl）-2-（4- chlorophenyl）-3-methylbutanamide

A novel compound N-（pyridine-2-methyl）-2-（4-chlorophenyl）-3-methylbutanamide, a racemic compound, has been synthesized with 2-（4-chlorophenyl）-3-methylbutyric acid and pyridin- 2-methylanamine as the raw materials, and its crystal structure （C17H19C1N2O, Mr = 302.79） was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/n with a = 9.624（9）, b = 23.14（2）, c = 15.626（15）A, β = 106.199（14）°, V = 3342（5） A^3, Z = 8, Dc = 1.204 g/cm^3,μ = 0.23 mm^-1, F（000） = 1280, S = 1.032, R = 0.0681 and wR = 0.1508 for 6513 unique reflections （Rint = 0.0421） with 3375 observed ones. In the crystal structure, there are some intermolecular hydrogen bonds which stabilize the crystal structure. The preliminary bioassay shows that the title compound exhibits good antifungal activity against Botrytis cinerea, Gibberella zeae, Dothiorella gregaria and Colletotrichum gossypii.     

Preparation,Crystal Structure and Theoretical Calculation of N-（Pyrimidin-2-yl）-N＇-methoxycarbonyl-thiourea

The compound, N-（pyrimidin-2-yl）-N＇-methoxycarbonyl-thiourea, has been synthesized. The single crystal structure has been determined by an X-ray diffractometer. The crystal belongs to triclinic with space group P-1 and a=0.72152（4） nm, b=0.8056（4） nm, c=0.90772（5） nm, α= 105.141（4）°, β=94.588（4）°, γ= 115.415（4）°, F（000）= 220, the unit cell volume V=0.45704（4） nm^3, the molecule number in one unit cell Z=2, the absorption coefficient μ=0.333 mm^-1, the calculated density Dc= 1.542 g/cm^3. The theoretical investigation of the title compound was carried out with B3LYP/6-311G, HF/6-311G and MP2/6-311G methods, and the atomic charges and natural bond orbital analysis were also discussed.     

Synthesis and Crystal Structure of （E）2-（3′-Bromo- 5′-chloro-salicylidene amino）-4-methyl Pyridine

A new Schiff base compound, 2-bromo-4-chloro-6-[（4-methylpyridin-2-ylimino）methyl]phenol （C13H10BrClN20）, has been synthesized by the condensation of equimolar 3-bromo-5- chlorosalicylaldehyde and 4-methylpyridin-2-ylamine in a methanol solution. The compound was characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21 with a = 6.048（3）, b = 14.063（7）, c = 7.623（4） A,β = 97.703（7）°, Z = 2, V = 642.5（6）A3, Dc = 1.683 g/cm3, Mr=325.59, 2（MoKa） = 0.71073A,μ = 3.395 mm^-1, F（000） = 324, R = 0.0370 and wR = 0.0662. A total of 3879 reflections were collected, of which 1970 with I 〉 2σ（I） were observed. As expected, the molecule adopts a trans configuration about the C=N double bond. The benzene and pyridine rings are nearly coplanar （mean deviation from the combined plane is 0.031（3）A）, with their dihedral angle of 3.3（3）°. The preliminary biological tests show that the compound has excellent antibacterial activities.     

Synthesis and Crystal Structure of 3-{[（1E） 1-（2- Hydroxyphenyl） methylidene]amino}-4-cyanopyrazole

The title Schiff base compound （C11H8N4O）, a derivative of pyrazole, has been synthesized by the reaction of salicylaldehyde and 3-amino-4-cyanopyrazole in absolute ethanol and characterized by elemental analyses, IR, ^1H NMR and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/n, with a = 7.5594（7）, b = 18.3342（19）, c = 22.461（2） A^°, β = 98.419（2）°, V = 3079.5（5） A^°3, Mr = 212.21, Z = 12, F（000） = 1320, Dc = 1.373 g/cm^3, T = 298（2） K, 2 = 0.71073 A^°, the final R = 0.0571 and wR = 0.0493. A total of 5412 unique reflections were collected, of which 1612 with I 〉 2σ（I） were observed. The molecular structure adopts a trans configuration about the C=N double bond. The preliminary biological tests show that the compound has high antibacterial activities.     

Synthesis,Crystal Structure and Biological Activities of 1-（（5-（4-（4-Chlorophenoxy）-2-chlorophenyl）-2,2,3- trimethyloxazolidin-5-yl）methyl）-1H-1,2,4-triazole

The title compound 1-（（5-（4-（4-chlorophenoxy）-2-chlorophenyl）-2,2,3-trimethyl-oxazolidin- 5-yl）methyl）-lH-1,2,4-triazole （C21H22Cl2N4O2）has been synthesized and characterized by elemental analysis, IR, 1H NMR, MS and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.891（2）, b = 9.074（2）, c = 18.258（4）AA, α = 99.292（4）, β = 95.105（4）, γ = 108.068（3）°, C21H22Cl2N4O2, Mr = 433.33, V= 1059.3（4） Aa, Z = 2, Dc = 1.359 g/cm3, F（000） = 452,μ = 0.331 mm-1, the final R = 0.0448 and wR = 0.0994 for 3727 unique reflections. The dihedral angle between the oxazolidine ring taking an envelope conformation with a local pseudo-mirror and the triazole ring is 27.7（9）°. Weak intermolecular C-H...N hydrogen bonds and π-π interactions exist between the triazole rings of neighboring molecules, forming a three-dimensional network, which stabilizes the crystal structure. The primary biological test shows the target compound has certain fungicidal activity.     

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 5-[（1H-1,2,4-Triazol-1- yl）methyl]-4-（2,3-dimethoxybenzylideneamino）-2- 2H-1,2,4-triazole-3（4H）-thione Monohydrate

1 INTRODUCTION Heterocyclic compounds bearing the 1,2,4-tri- azole moiety have attracted considerable attention over the past few decades since they exhibit some fungicidal activities against Puccinia recondite and applications in the field of root-growth regu- lation[1~3]. Meanwhile, 4-amino-5-mercapto-1,2, 4-triazole moiety has great versatility in fusing tovarious ring systems and possesses a broad spec- trum of biological activities[4, 5]. In our con- tinuous work directed towards the…     

Synthesis, Crystal Structure, Antibacterial Activities and Theoretical Computation of 3-（2-Hydroxybenzly）-4-（4-isopropylbenzylideneamino）-（1H）-1,2,4-triazole-5-thione

1INTRODUCTION Recently,compounds containing pyrazole,imida-zole,triazole(including benzotriazole),pyridine,tetrazole and indole have attracted much interest because they exhibit some fungicidal activity,plant-growth regulating activity and antibacterial acti-vity[1～10].Schiff bases also constitute a good type of biologically active substructure[11～14],and the sulfur-containing Schiff bases are particularly effective.Studies of pyrazole Schiff base-type fungicides andtriazole compounds c…     

Synthesis and Crystal Structure of Trans-4-[(5-(2,4-Dichlorophenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one

The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl-1-phenyl-1H-pyra-zol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6) , α = 112.566(1), β = 92.324(2), γ = 102.91(1)o, V = 1315.65(10) 3, Z = 2, Dc = 1.344 g/cm3, μ(MoKα) = 0.282 mm-1, λ = 0.71073 , F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I > 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra-and intermolecular C(12)-H(12)···O(1) and C(28)-H(28)···O(1)#1 hydrogen bonds were observed in the title compound.     

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, Crystal Structure and Herbicidal Activity of N-（7-Chloro-5-ethoxy-2H-[1,2,4] thiadiazolo [2,3-a] pyrimidin-2-ylidene）-2-（2,4-dichlorophenoxy）propanamide

The title compound N-(7-chloro-5-ethoxy-2H-[1,2,4]thiadiazolo[2,3-a]pyrimidin- 2-ylidene)- 2-(2,4-dichlorophenoxy)propanamide 3 has been synthesized through using bromine as cyclic reagent in 63% isolated yield. Suitable single crystals for X-ray diffraction were obtained by recrystallization from the mixture solvents at room temperature. Crystallographic data of 3: C16H13- Cl3O3S, Mr = 447.71, triclinic, space group P, a = 8.7461(8), b = 9.9560(10), c = 11.8572(11) , α = 94.341(2), β = 94.683(2), γ = 112.929(2)o, Z = 2, V = 941.21(15) 3, Dc = 1.580 g/cm3, F(000) = 456, R = 0.0794, wR = 0.2056 and μ(MoKα) = 0.623 mm-1. The title compound 3 was found to be effective in herbicidal activity.     

Syntheses and Crystal Structures of 4-Amino-3- （3-hyd roxyp ropyl）- 1H-1,2,4-triazole-5（4H）-thione and 6-（4-Biphenylyl）-3-（3-hydroxypropyl）-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine

1INTRODUCTION It has been reported that3,6-disubstituted-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazines have a broad spec-trum of bioactivities,such as antimicrobial[1],antibac-terial,antifungal[2],anti-inflammatory[3],diuretic[4],an-thelmintic and analgesic[5].They can also be used as plant-growth regulating agents[6],photographic coup-lers,dyes for improved preservability and absorption characteristics,and inhibitors of malignant cellularZOU K.H.et al.:Syntheses and Crystal Structures o…     

Synthesis and Crystal Structure of 3-Phenyi- 6-（4-methylphenyi）-1,2,4-triazolo[4,3-b]-1,2,4-triazine

1 INTRODUCTION The fused heterocycles bearing 1,2,4-triazine have attracted considerable attention in recent years owing to their biological and pharmaceutical activi- ties[1～3]. The 1,2,4-triazine core is a versatile synthe- tic platform to access a wide range of condensed heterocyclic ring systems via inter- and intramolecu- lar Diels-Alder reaction with a vast array of dieno- philes[4～6]. IBD (iodobenzene diacetate) is commer- cially available and used as benign non-metallic oxidant…     

Crystal Structure and DFT Studies of a Triazole Derivative： 4- （ 2-Hydrobenzylideneamino ） -3- （ 1,2,4-triazol-4-ylmethyl） 1H-1, 2,4-triazole-5 （4H） -thione

A novel triazole derivative 4-(2-hydrobenzylideneamino)-3-(1,2,4-triazol-4-ylmethyl)-1H-1,2,4-triazole-5(4H)-thione(1) was synthesized and characterized using elemental analysis, FTIR, and 1H NMR, and its crystal structure was determined via X-ray single crystal diffraction analysis. Crystal data: monoclinic, P2(1)/c, a=0.83335(9) nm, b=1.49777(16) nm, c=1.14724(12) nm, β =107.990(2)°, D=1.470 Mg/m3, and Z=4. The geometries and the vibrational frequencies were determined using the density functional theory(DFT) method at the B3LYP/ 6-31G level. To demonstrate the accuracy of the reaction route of compound 1, one of the important intermediates was also tested using the same method. The structural parameters of the two compounds calculated using the DFT study are close to those of the crystals, and the harmonic vibrations of the two compounds computed via the DFT method are in good agreement with those in the observed IR spectral data. The thermodynamic properties of the title compound were calculated, and the compound shows a good structural stability at normal temperature. The test results of biological activities show that it has a certain bactericidal ability.     

Synthesis and Crystal Structure of 4-Phenyl-5-(1′- t-butyl-5′-methyl-4′-pyrazolyl)-1,2,4-triazol-3-thione

The crystal structure of 4-phenyl-5-(1′-t-butyl-5′-methyl-4′-pyrazolyl)-1,2,4-triazol- 3-thione 5 (C16H19N5S, Mr = 313.42) has been determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 6.680(2), b = 27.44(1), c = 9.388(4)(A。), β = 106.738(6)°, V = 1648(1)(A。)3, Z = 4, Dc = 1.263 g/cm3, μ= 0.200 mm-1, F(000) = 664, R = 0.0608 and wR = 0.1176. The results confirmed that 5 can be assigned to the thione tautomeric form.