Synthesis,X-ray Structure aSynthesis,X-ray Structure and Bioactivity of N-4-Methyl-1,2,3-thiadiazole-5-carbonyl-N′-3,5- dichloro-4-(1,1,2,2-tetrafluoroethoxyl)phenyl Urea

The title compound N-4-methyl-1,2,3-thiadiazole-5-carbonyl-N?-3,5-dichloro-4- (1,1,2,2- tetrafluoroethoxyl)phenyl urea (C13H8Cl2F4N4O3S, Mr = 447.19) has been synthesized from 4-methyl- 1,2,3-thiadiazole-5-carbonyl chloride as the starting material, and its structure was characterized by proton Nuclear Magnetic Resonance (1H NMR), Infra Red Spectroscopy (IR), high-resolution mass spectroscopy (HRMS), and single-crystal X-ray diffraction. The crystal of the title compound belongs to triclinic, space group P with a = 6.0780(8), b = 11.3760(14), c = 12.1440(18) , α = 96.887(7), β = 91.027(12), γ = 104.252(13)°, Z = 2, V = 806.98(19) ·3, Dc = 1.840 g/cm3, μ = 0.601 mm-1, F(000) = 448, R = 0.0450 and wR = 0.0869. X-ray analysis indicates that the 1,2,3-thiadiazole ring is not coplanar with the phenyl ring, and the dihedral angle is 33.57°. Two intermolecular hydrogen bonds N(2)-H…O(1), S(1)…H-C(11), and three weak intermolecular interactions, C(11)…O(1), N(1)…O(2) and S…O(1), are observed. The bioassay results indicate that the title compound has good insecticidal activity against Culex pipiens pallens and good induction activity for tobacco against tobacco mosaic virus which is equal to that of TDL.     

Synthesis,Crystal Structure,and Biological Activity of Naphthalen-2-yl4-methyl-1,2,3-thiadiazole-5-carboxylate

The title compound naphthalen-2-yl-4-methyl-1,2,3-thiadiazole-5-carboxylate (C 14 H 10 N 2 O 2 S,M r=270.31) was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its structure was characterized by IR,1 H NMR,high-resolution mass spectrometry and single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group Pbcn with a=23.475(5),b=9.6640(19),c=10.814(2),β=90.00°,Z=8,V=2453.2(9) 3,M r=270.30,D c=1.464 g/cm 3,μ=0.262 mm-1,F(000)=1120,R=0.0444 and wR=0.1099.X-ray analysis revealed that the thiadiazole and naphthalene rings were non-planar,while the thiadiazole ring and the ester group were essentially planar,and two intermolecular hydrogen bonds C(6) H(6)···O(1) and C(14) H(14)···O(1) were observed.The preliminary biological test showed that the title compound had antifungal and antivirus activities against tobacco mosaic virus.     

Synthesis, Crystal Structure, and Biological Activity of N-（ （ 1-cy clo h e xyl- 1H-tetrazo l-5-yl）（ 5-methyl- 1,2,3- thiadiazol-4-yl）methyl）-4-nitrobenzenamine

The title compound N-((1-cyclohexyl-1H-tetrazol-5-yl)(5-methyl-1,2,3-thiadiazol-4-yl) methyl)-4-nitrobenzenamine (C17H20N8O2S, Mr = 400.47) was synthesized via Ugi fourcomponents condensation reaction (U-4CR), and its structure was characterized by IR, 1H NMR, high-resolution mass spectrometry and single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pna21 with a = 20.390(2), b = 12.9660(14), c = 6.9399(8) , β = 90.00°, Z = 4, V = 1834.7(3)3, Mr = 400.47, Dc = 1.450 g/cm3, μ = 0.210 mm-1, F(000) = 840, R = 0.0348 and wR = 0.0717. X-ray analysis reveals that the dihedral angles formed between the thiadiazole and tetrazole rings, the benzene and tetrazole rings and the thiadiazole and benzene rings are 62.59, 86.73 and 70.07°, respectively. Three intermolecular hydrogen bonds N(1)-H(2)···N(6), C(4)-H(4B)···O(2) and C(17)-H(17)···N(3) are observed. Bioassay shows that the title compound has antifungal and antivirus activities against tobacco mosaic virus.     

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 Cis-syn Cyclobutane 1-（Carboxyethyl）thymine Dimer Monopentyl Amide Monotryptophan Methyl Ester Amide

The crystal structure of the title compound (C34H47N7O9, Mr = 697.79) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21 with a = 9.000(8), b = 11.360(10), c = 17.841(15) , β = 97.083(14)°, V = 1810(3) 3, Z = 2, F(000) = 744, Dc = 1.280 g/cm3, μ = 0.094 mm-1, the final R = 0.0721 and wR = 0.1942 for 2479 observed reflections with I > 2σ(I). The two methyl groups attached to the cyclobutane ring are cis oriented. An intramolecular hydrogen bond (N(6)-H(6)…O(8)) introduces rigidity into the title molecule and the crystal structure is stabilized by intermolecular N-H…O hydrogen bonds.     

Synthesis and Crystal Structure of 3,6-Bis（4-methyl-1,2,3-thiadiazol-5-yl）-1,2,4-triazolo[3,4-b][1,3,4]thiadiazole

The compound 3,6-bis(4-methyl-1,2,3-thiadiazol-5-yl)-1,2,4-triazolo[3,4-b][1,3,4] thiadiazole(C9H6N8S3,Mr = 322.40) has been synthesized by the reaction of 4-amino-3-(4-methyl-1,2,3-thiadiazolyl)-5-mercapto-1,2,4-triazole with 4-methyl-1,2,3-thiadiazol-5-carboxylic acid and phosphorus oxychloride,and its structure was characterized by IR,1H NMR,EI-MS,elemental analysis and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic,space group C2/c with a = 2.0053(4),b = 1.3081(3),c = 1.0556(2) nm,β = 112.69(3)°,Z = 4,V = 2.5548(9) nm3,Dc = 1.676 g/cm3,μ = 0.582 mm-1,F(000) = 1312,R = 0.0546 and wR = 0.1523.X-ray analysis indicates that all rings are essentially planar in this molecule,and an intermolecular hydrogen bond C(9)-H(9)…N(2) and weak intramolecular interactions between S(1)…N(7),S(3)…N(1) and S(2)…N(4) are observed.     

Synthesis,Crystal Structure and Herbicidal Activity of O,O＇-Diethyl-N-[2-（5,7-dimethyl-[1,2,4]triazolo[1,5-a]pyrimidin-2-yloxy）-benzoxyl]-1-amino-benzyl phosphonate

The crystal structure of the title compound (C25H28N5O5P,Mr=509.49) has been determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P21/c with a=13.0726(4),b=13.4513(4),c=15.103(1),β=93.650(1)°,V=2650.29(14)3,Z=4,Dc= 1.277 g/cm3,F(000)=1072,μ(MoKα)=0.147 mm-1,the final R=0.0748 and wR=0.1956 for 3186 observed reflections (I 2σ(I)).The fused triazolopyrimidine system ring is coplanar,the dihedral angles between the triazolopyrimidine and C(1)-C(3)-C(5) phenyl,the triazolopyrimidine and C(17)-C(19)-C(21) phenyl,and the two phenyl rings are 66.87,58.79 and 80.11o,respectively.Intramolecular N(5)-H(5A)…O(3) and intermolecular C(2)-H(2)…N(4),C(18)-H(18)…O(3),C(19)-H(19)…O(2) and C(24)-H(24C)…N(4) hydrogen bonds together with C-H…π interactions contribute to the stability of the structure and result in a three-dimensional framework.The preliminary bioassay indicates that the title compound exhibits moderate herbicidal activity against dicotyledonous plants (Brassica campestris L) at the concentration of 100 mg/L.     

Synthesis and Crystal Structure of Spiro[1-bromo-4- methoxy-5-oxa-6-oxo-bicyclo[3.1.0]hexane-2,2''-(3''- cyclohexanoxy-4''-methoxybutyrolactone]

The crystal of the title compound 6 has been prepared and determined by X-ray diffraction analysis. It belongs to the orthorhombic system, space group P212121 with a = 10.195(2), b = 11.955(2), c = 14.335(3)(A), C16H21BrO7, Mr = 405.24, V = 1747.0(6) (A)3, Z = 4, Dc = 1.541 g/cm3, μ = 2.387 mm-1, F(000) = 832, R = 0.0266 and wR = 0.0348 for 2110 observed reflections with I > 2σ(I). The crystal exhibits a characteristic spiral structure consisting of one cyclopropane and two butyrolactones with envelope configuration. The intermolecular hydrogen bond between C(16)- H(16)…O(1) and C(3)-H(3)…O(2) has been observed in the crystal lattice.     

Synthesis and Structure of 5-Amino-6-(4-fluorophenylamino)-3-methylthio-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one

The title compound (C18H15FN6OS) has been synthesized and its crystal structure was determined by X-ray analysis. The crystal belongs to monoclinic system, space group P21/n with a = 13.983(10), b = 7.337(5), c = 16.702(12) (A), α = 90, β = 98.277(12), γ = 90°, V = 1696(2)(A)3, Z = 4, Dc= 1.498 g/cm3, Mr = 382.42,μ = 0.224 mm-1, F(000) = 792, the final R = 0.0362 and wR = 0.0878 for 2579 observed reflections with I ＞ 2σ(Ⅰ). In the title compound, the atoms of C(1),C(2), C(3), C(4), C(5), N(1), N(2), N(3), N(4), N(5), N(6), O(1) and S(1) form a fully delocalized system with the average deviation of 0.0307(A). There exists a part of electron delocalization over the planes of Ⅰ (pyrazolo[3,4-d]pyrimidin-4-one moiety), Ⅱ (phenyl moiety) and Ⅲ (p-fluorophenylamine moiety). In the molecule, intermolecular hydrogen bonds between N(6)-H(6)…O(1)and C( 15)-H( 15)…O( 1 ) are observed.     

Synthesis and Crystal Structure of S-（＋）-N＇-Tertbutylaminocarbonyl-N- [3-methyl-2-（4-chlorophenyl）butyryl] Thiourea

The title compound S-( )-N'-tertbutylaminocarbonyl-N-[3-methyl-2-(4-chlorophenyl)butyryl] thiourea has been synthesized and its crystal structure was determined by singlecrystal X-ray diffraction an alysis. There exist intramolecular N(2)-H(2A)… O(1), C(17)-H(17A)…O(2) and N(3)-H(3A)…S(1) hydrogen bonds as well as intermolecular N-H…O interaction between the carbonyl and amidogen groups. Crystallographic data: C17H24ClN3O2S, Mr = 369.90,monoclinic, space group C2/c with a = 22.9922(19), b = 14.4844(12), c = 12.4618(11) (A),β =92.608(2)°, V= 4145.8(6) (A)3, Z = 8, Dc = 1.185 g/cm3, F(000) = 1568,μ(MoKa) = 0.298 mm-1, R =0.0578 and wR = 0.1308.     

Synthesis and Crystal Structure of （E）-ethyl 6-benzyl-2-[（cyclopropylmethylamino）（4-fluorophenylamino）-methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate

The crystal structure of the new title compound (E)-ethyl 6-benzyl-2-[(cyclopropylmethylamino)(4-fluorophenylamino)methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate (C28H31FN 4O2S·C2H6O, Mr=552.70) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a=13.806(10), b=10.850(7), c=19.938(14), β=98.842(9)° , V=2951(4)3 , Z=4, Dc=1.244g/cm 3 , F(000)=1176, μ=0.153 mm-1 , MoKα radiation (λ=0.71073), R=0.0758 and wR=0.2234 for 4262 observed reflections with I > 2σ(I). Intramolecular N-H…S and C-H…N interactions as well as intermolecular N-H…O and O-H…N hydrogen bonds help to stabilize the crystal structure. X-ray diffraction analysis reveals that the asymmetric unit contains one title molecule and one ethanol molecule.     

Synthesis and Crystal Structure of N-(1,3,4-Thiadiazol-2-yl)-1-[1-(6-chloropyridin-3-yl)methy]-5-methyl-1H-[1,2,3]triazol-4-carboxamide

The crystal structure of the title compound (C12H10ClN7OS,Mr=335.78) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic,space group P1 with a=8.4093(11),b=9.4430(12),c=11.1454(14),α=95.508(2),β=111.366(2),γ=115.259(2)°,V=711.42(16) 3,Z=2,Dc=1.568 g/cm3,F(000)=344,μ(MoKα)=0.428 mm-1,the final R=0.0476 and wR=0.1243 for 2353 observed reflections (I > 2σ(I)). The dihedral angles between the pyridine and triazole,thiazole and triazole,and pyridine and thiazole rings are 69.2(1),9.2(1) and 72.7(1)o,respectively. Intramolecular C(8)-H(8B)…O(1) and N(5)-H(5A)…N(4) as well as intermolecular C(5)-H(5)…S(1),C(3)-H(3)…N(6) and N(5)-H(5A)…N(1) hydrogen bonds together with weak C-H…π hydrogen-bonding and π-π stacking interactions contribute to the stability of the structure. There is also evidence for significant electron delocalization in the triazolyl system.     

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 2-[（4-Methoxy- 6-methylthio-2-pyrimidinyl）aminocarbonyl- aminosulfonyl] Benzoic Acid Methyl Ester

1 INTRODUCTION The sulfonylurea herbicides are characterized by broad-spectrum weed control at very low use rates (c.2~75g ai ha-1), good crop selectivity and very low acute and chronic animal toxicity (acute oral LD50 to rat >4000 mg/kg)[1]. They are e…     

Synthesis and Crystal Structure of (4R, 5R)(5-Hydroxymethyl-2,2-dimethyl- [1,3]dioxolan-4-yl)-bis-(4-methoxy-phenyl)-methanol

1　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅα ,α ,α′,α′ ｔｅｔｒａａｒｙｌ 1 ,3 ｄｉｏｘｏｌａｎｅ 4,5 ｄｉｍｅｔｈａｎｏｌｓ (ＴＡＤＤＯＬＳ)ｄｉｏｌｓｗｈｉｃｈａｒｅｒｅａｄｉｌｙａｖａｉｌａｂｌｅｆｒｏｍａｌｋｙｌｔａｒｔｒａｔｅｓ ,ｈａｖｅｂｅｅｎｗｉｄｅｌｙｕｓｅｄａｓｃｈｉｒａｌｌｉｇａｎｄｓｉｎｅｎａｎｔｉｏｓｅｌｅｃｔｉｖｅａｄｄｉｔｉｏｎｒｅａｃｔｉｏｎｓｏｆｃａｒｂｏｎ ｃｅｎｔｅｒｅｄｎｕｃｌｅｏｐｈｉｌｅｓｔｏａｌｄｅｈｙ ｄｅｓ[1 ] ,ｉｎ [2 +2 ]ｃｙｃｌｏａｄｄｉｔｉｏｎｓ[2 ] …     

Synthesis and Structure of N-（1,5-Dihydro-1-phenyl-3-methyl-4-benzoyl）-3-chloroaniline

1 INTRODUCTION 4-Acyl-5-pyrazolone, a family of flexible b- diketonate, is widely used as extract[1] and well known for its applications as analgesics, antipyre- tics, anti-inflammatory and insecticides[2]. Therefore the study on the derivation of 4-acyl-5-pyrazolone is the focus of many research groups working in the fields of coordination chemistry, biomedicine and pharmaceutical chemistry. In order to study the rela- tionship between the structure and performance of these compounds, w…     

Synthesis and Crystal Structure of Bis（p—aminotoluene）—bis（dimethylglyoximato） Cobalt（Ⅲ） Perchlorate

The title compound (C22H32.5ClCoN6O8.25,Mr=607.42)crystallizes in the orthorhombic system,space group c222 1 with a=11.320(2),b=20.933(4),c=23.936(5)A,V=5672(2)A^3,Dc=1.423g/cm^3,Z=8,μ(MoKα）=0.754mm^-1,F(000)=2532,R=0.0512 and wR=0.1190,There are eight complex molecules [Co(C4H6N2O2)(C4H8N2O2)(C7H9N)2]ClO4.0.25H2O of C2 crystallographic symmetry in a unit cell,including two crystallographically independent molecules,in which different orientations of the MePhNH2 groups are found.Two MephNH2 groups are in trans position for molecule A,and cis for B.The central metal atom is in a distroted octahedral environment.The hydrogen bonds of O-H(oxime)…O and N-H(p-aminotoluene group)…O construct an one-dimensional chain along the c axis in the title compound.     

三维超分子化合物[H_2(C_4H_(10)N_2)](SO_4)(H_2O)的制备、晶体结构及差热-热重性质研究

用MnSO4H2O和哌嗪在水-甲醇混合溶剂中反应得到了1个超分子化合物[H2(C4H10N2)](SO4)(H2O) (C4H14N2O5S)。 该晶体属单斜晶系, 空间群为P21/n, 晶胞参数为: a = 6.386(1), b = 11.695(2), c = 11.680(2) ? = 101.06(3), V = 856.1(3) 3, Z = 4, Mr =202.23 , Dc = 1.569 g/cm3, F(000) = 432, ?= 0.368 mm-1。 该化合物是由[H2(C4H10N2)]2+、SO42-、H2O通过氢键自组装而形成的。 其中[H2(C4H10N2)]2+存在2种椅式构象:一种[H2(C4H10N2)]2+与4个SO42-、2个H2O通过氢键相连, 另一种[H2(C4H10N2)]2+则与6个SO42-相连。 它们分别沿着b、c方向交替排列展开, 通过SO42-桥联成二维的层状结构;层与层之间在NH…O、CH…O、OH…O氢键的作用下互相连接, 形成了具有网状结构的三维超分子化合物。 差热及热重测试表明:该化合物从92℃开始分解,首先失去1个H2O, 然后再失去[H2(C4H10N2)]2+和SO4 2-。     

Synthesis,Spectroscopic Properties and Crystal Structure of 3,3＇-（Anthracene-9,10-diyl）bis（1-phenylpropan-1-one）

The compound 3,3'-(anthracene-9,10-diyl)bis(1-phenylpropan-1-one)(C32H26O2,Mr=442.55) has been synthesized by the reaction of 2,2'-(anthracene-9,10-diylbis(methy-lene))bis(1,3-diphenylpropane-1,3-dione) with CsCO3,and its structure was characterized by 1H NMR and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic,space group P21/c with a=9.154(3),b=5.2777(16),c=24.897(7) nm,β=107.337(10)°,Z=2 and V=1.1482 nm3.X-ray analysis indicates that an intermolecular hydrogen bond C(8)-H(8A)…O(1),weak C-H···π between H(9A) and the centre of anthracene rings and weak π-π interactions between two anthracene ring planes are observed.     

Synthesis,Crystal Structure and Characterization of a Cobalt Coordination Polymer： [Co（1,4-ndc）（L） （H2O）]n

The title coordination polymer, [Co（1,4-ndc）（L）（H2O）]n 1 （1,4-H2ndc = 1,4-na- phthalenedicarboxylic acid and L =1-（5-（1H-imidazol- 1-yl）pentyl）- 1H-imidazole） has been hydrothermally synthesized and characterized by IR and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.4333（12）, b = 13.2963（13）, c = 13.4678（13）A, α =β = 90°, y =107.302（2）°, V= 2125.7（4）A^3, Z = 4, CoC22H22N4O5, Mr = 481.37, De = 1.504 g/cm^3, F（000） = 996, μ（MoKa） = 0.850 mm^-1, R = 0.0472 and wR = 0.0984. Compound 1 exhibits a two-dimensional layer structure. The O-H...O and C-H...O hydrogen bonds stabilize the structure of 1.