Synthesis,Crystal Structure and Biological Activity of N-（2,6-Difluorobenzoyl）-N＇-[5-（4-trifluoromethyl-phenyl）-1,3,4-thiadiazol-2-yl]ure

The title compound N-(2,6-difluorobenzoyl)-N'-[5-(4-trifluoromethylphenyl)-1,3,4-thiadiazol-2-yl]urea(C17H9F5N4O2S,Mr = 428.34) has been synthesized by the reaction of 2-amino-5-(4-trifluoromethylphenyl)-1,3,4-thiadiazole with 2,6-difluorobenzoyl isocyanate,and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/n with a = 10.7316(13),b = 10.5617(13),c = 16.037(2) ,β = 106.408(2)°,V = 1743.6(4) 3,Z = 4,Dc = 1.632 g/cm3,μ = 0.260 mm-1,F(000) = 864,the final R = 0.0599 and wR = 0.1420 for 3467 observed reflections with I > 2σ(I).The urea group,which adopts a planar configuration mediated by the intramolecular N-H...O hydrogen bond,is nearly coplanar with the thiadiazole and 4-trifluoromethylbenzene rings.The title compound was found to exhibit good fungicidal activity against Rhizoctonia solani and Botrytis cinerea.     

Synthesis, Dimeric Crystal Structure, and Biological Activities of N- （ 4-Methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl ） -N＇- （ 2-trifluoromethyl-phenyl ） -guanidine

The title compound, N-（4-methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl）-N＇-（2-tritluoromethyl-phenyl）-guanidine, was synthesized and its structure was confirmed by using IR, MS,^1H NMR, and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test showed that the synthesized compound has a weak herbicidal activity.     

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,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, Structure and Biological Activities of 2- （4-Met hoxybenzoyl ）-N-phenyl- 2- （ 1,2,4-triazol- 1-yl ） thioacetamide

The title compound, 2-(methoxybenzoyl)-N-phenyl-2-(1,2,4-triazol-l-yl) thioacetamide was synthesized by several reactions from 4-methoxyacetophenone, triazole and phenyl isothiocyanate. The structure was identified by elemental analysis, ^1H NMR, MS and IR. The single crystal structure of 2-(methoxybenzoyl)-N-phenyl-2-(1,2,4-triazol-l-yl)thioacetamide was determined withX-ray diffraction. The preliminary bioassays show that the title compound exhibits weak antifungal activities and plant-growth regulatory activity.     

Synthesis, Crystal Structure, and Biological Activities of 2-Oxo-2-aryl-1 - （ 1,2,4-triazol-1 -yl ） ethyl phenylcarbamodithioate

IntroductionAs an important type of fungicide, compoundscontaining 1,2,4-triazole groups have attracted muchattention because they exhibit a certain fungicidal acti-vity againstPuccinia reconditeand also play a role inroot-growth regulation[1—3]. However…     

Synthesis and Crystal Structure of 4-（4,6-Dimethoxylpyrimidin-2-yl）- 3-thiourea Carboxylic Acid Ethyl Ester

4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.     

Synthesis, Crystal Structure and Biological Activities of N＇ - （ 4-Methoxybenzylidene ） -2- （ 1H-1, 2,4- triazol-1-yl） acetohydrazide

The title compound, N‘-( 4-methoxybenzylidene ) -2-( IH-1, 2,4-triazol-1-yl ) acetohydrazide, was synthesized and its structure was confirmed by means of IR, MS,^1H NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test shows that the synthesized compound has a low antifungal activity.     

Synthesis and Crystal Structure of a Copper（Ⅱ） Compound Constructed by N-（4,6- Dimethoxylpyrimidin）-N＇-（ethoxycarbonyl）thiourea

A copper（Ⅱ） complex Cu（L）2（NO3）2 constructed by the L （L = N-（4,6-dimethoxylpyrimidin）-N＇-（ethoxycarbonyl）thiourea） ligand crystallizes in monoclinic, space group C2/c with a = 16.2416（16）, b = 9.1385（7）, c = 22.0008（18） A, β = 108.077（2）°, V = 3104.3（5） A^3, Dc = 1.627 g/cm^3, Z = 4, C20H28CuN10O14S2, Mr = 760.18,μ（MoKa） = 0.920 mm^-1, F（000） = 1564, R = 0.0471 and wR = 0.1284 for 2239 observed reflections （I 〉 2σ（I））. X-ray diffraction shows the existence of weak complementary intramolecular N-H...O （DA） hydrogen bonds which further strengthen the coordination from the two L ligands with the Cu（Ⅱ） ion, intermolecular C-H...O hydrogen bonds and weak π...π stacking interactions, leading to the formation of a multi-dimensional supramolecular network.     

Synthesis and Crystal Structure of Sodium Monosulfuron （N-（4-Methylpyrimidin-2-yl）-N＇-2-（nitrophenylsulfonyl） Urea Sodium）

ABSTRACT Monosulfuron is a novel sulfonylurea herbicide with ultra-low dosage invented and patented by Nankai University. Herein its sodium salt was firstly synthesized and crystal structure was determined by X-ray diffraction method. The title compound belongs to the triclinic system, space group P1^- with a = 7.306（6）, b = 9.446（8）, c = 11.872（10）A, α = 76.578（14）, β = 78.049（13）, γ = 77.620（14）°, V = 767.7（11）A^3, Mr = 377.32, Z = 2, Dc = 1.632 g/cm^3,μ= 0.283 mm^-1, F（000） = 388, R = 0.0444 and wR = 0.1186. In the title compound, Na（1） coordinates with 0（4） and 0（5） from one monosulfuron molecule, N（4A） and O（5A） from the other monosulfuron molecule and the oxygen atom from H2O to give five coordination bonds. The title complex is further linked into a three-dimensional structure through π…π interactions and intermolecular hydrogen bonds between the oxygen and nitrogen atoms.     

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 (C19H14ClF3N4O2S) 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) , β = 98.058(9)°, V = 1986(2) 3, Mr = 454.85, Z = 4, Dc = 1.521 g/cm3, 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 herbicidal activity for the title compound.     

N'(4,6-二甲基嘧啶-2-基)苯甲酰硫脲的晶体结构及除草活性

经对N?(4,6-二甲基嘧啶-2-基)苯甲酰硫脲进行初步生物活性测定结果表明,该化合物具有除草活性,现经除草活性复筛测试发现,它主要抑制阔叶杂草的生长,对禾本科作物较安全。为了进一步了解该类化合物除草活性与结构的关系,也为设计新的除草剂分子提供帮助,对标题化合物进行了X射线单晶衍射,它的晶体结构数据为分子简式C14H14N4OS,分子量为286.35,三斜晶系,空间点群为P,a=8.216(1),b=9.503(1),C=9.942(11)?a=74.995(2),b=76.774(2),g=70.305,V=697.2(2)3,Z=2,DC=1.364g/cm3,F(000)=300,m(MoKa)=0.233mm-1,R=0.0457,wR=0.0965。     

N''''-(4,6-二甲基嘧啶-2-基)苯甲酰硫脲的晶体结构及除草活性

经对N?(4,6-二甲基嘧啶-2-基)苯甲酰硫脲进行初步生物活性测定结果表明,该化合物具有除草活性,现经除草活性复筛测试发现,它主要抑制阔叶杂草的生长,对禾本科作物较安全。为了进一步了解该类化合物除草活性与结构的关系,也为设计新的除草剂分子提供帮助,对标题化合物进行了X射线单晶衍射,它的晶体结构数据为分子简式C14H14N4OS,分子量为286.35,三斜晶系,空间点群为P,a=8.216(1),b=9.503(1),C=9.942(11)?a=74.995(2),b=76.774(2),g=70.305,V=697.2(2)3,Z=2,DC=1.364g/cm3,F(000)=300,m(MoKa)=0.233mm-1,R=0.0457,wR=0.0965。     

1-(4-甲氧基)苯甲酰基-3-(4,6-二甲基嘧啶-2-氨基)硫脲的晶体结构、 理论计算及生物活性

2-氨基-4,6-二甲基嘧啶与硫氰酸钾、4-甲氧基苯甲酰氯在乙酸乙酯中反应, 合成了1-(4-甲氧基)苯甲酰基-3-(4,6-二甲基嘧啶-2-氨基)硫脲, 并用X射线单晶衍射法测定其晶体结构, 晶体属单斜晶系, 空间群为P21/n, 晶胞参数为: a＝1.0134(4) nm, b＝1.3172(5) nm, c＝1.0988(4) nm, β＝91.671(8)°, V＝1.4661(9) nm3, Dc＝1.433 g/cm3, μ＝0.234 mm－1, F(000)＝664, Z＝4, R1＝0.0571, wR2＝0.1328. 运用Gaussian 03程序, 对标题化合物进行了HF/6-31＋g(d)和B3LYP/6-31＋g(d)水平的几何全优化和频率计算, 并对其成键情况及自然键轨道(NBO)进行了分析. 初步实验证明该化合物具有良好的生物活性.     

Synthesis, Crystal Structure and Biological Activity of N-(2,6-Difiuorobenzoyl)-N'-[5-(4-trifiuoromethylphenyl)-1,3,4-thiadiazol-2-yl] ure

The title compound N-(2,6-difluorobenzoyl)-N'-[5-(4-trifluoromethylphenyl)-1,3,4-thiadiazol-2-yl]urea(C17H9F5N4O2S, Mr = 428.34) has been synthesized by the reaction of 2-amino-5-(4-trifluoromethylphenyl)-l,3,4-thiadiazole with 2,6-difluorobenzoyl isocyanate, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 10.7316(13), b = 10.5617(13), c = 16.037(2) (A), β =106.408(2)°, V= 1743.6(4) (A)3, Z = 4, Dc = 1.632 g/cm3, μ = 0.260 mm-1, F(000) = 864, the final R = 0.0599 and wR = 0.1420 for 3467 observed reflections with I ＞ 2o(Ⅰ). The urea group, which adopts a planar configuration mediated by the intramolecular N-H…O hydrogen bond, is nearly coplanar with the thiadiazole and 4-trifluoromethylbenzene rings. The title compound was found to exhibit good fungicidal activity against Rhizoctonia solani and Botrytis cinerea.     

N-(4,6-二取代嘧啶-2-基)-N'-(1-甲基-3-乙基-4-氯吡唑-5-基)甲酰基(硫)脲的合成及生物活性

利用活性结构拼接原理,将高效杀螨剂吡螨胺分子的吡唑环部分引入酰基（硫）脲化合物中,以1-甲基-3-乙基-4-氯-5-甲酸基吡唑和2-氨基-4,6-二取代嘧啶为起始原料,通过多步反应合成了5种N-（4,6-二取代嘧啶-2-基）-N’-（1-甲基-3-乙基-4-氯吡唑-5-基）甲酰基脲和5个N-（4,6-二取代嘧啶-2．基）-N’-（1．甲基-3-乙基-4-氯吡唑-5-基）甲酰基硫脲化合物,其化合物结构经IR、^1HNMR及元素分析测试技术确证。初步生物活性试验表明,在50mg／L质量浓度下目标化合物的杀螨活性不太理想,但有些化合物具有较好的除草活性,其中化合物Ib、Ic和Ie对稗草主根的生长抑制率大于60％。     

N-取代芳酰氨基-5-氟代苯基-2-呋喃甲酰硫脲的合成与生物活性测定

从5-氟代苯基-2-呋喃甲酸出发, 经酰化、异硫氰酸酯化, 再与取代芳酰肼反应合成了20个未见文献报道的N-取代芳酰氨基-5-氟代苯基-2-呋喃甲酰硫脲. 目标产物的结构经IR, ¹H NMR和元素分析测定确证. 初步生物活性测试表明, 部分化合物对棉花枯萎病、黄瓜灰霉病、苹果轮纹病和棉花炭疽病有较好的选择性杀菌活性; 部分目标化合物有较好的除草活性.     

Synthesis,Crystal Structure and Biological Activity of 2-(1-(3-Bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbonyl)piperidin-4-yl)-N-isopropyl-1,3-thiazole-4-carboxamide

The title compound 2-(1-(3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbonyl)piperidin-4-yl)-N-isopropylthiazole-4-carboxamide(C21H22Br Cl N6O2 S,Mr = 536.04) has been synthesized,and its structure was characterized by IR spectra,1H-NMR,13C-NMR,EA,and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic system,space group P/c with a = 15.146(3),b = 11.573(2),c = 26.937(5) ?,β = 103.64(3)°,V = 1839.0(6) ?3,Z = 4,Dc = 1.557 g/cm3,μ(Mo Ka) = 0.71073 mm-1,F(000) = 2192,R = 0.0601 and w R = 0.1392.There exist one intramolecular hydrogen bond at N–H···N and four intermolecular weak interactions at O(2)···H(1),Cl(1)···H(12),O(1)···Cl(1) and S(1)···O(2).Bioassay results indicated that the title compound had good fungicidal and antiviral activities against tobacco mosaic virus.     

Synthesis,Crystal Structure and Biological Activity of 2-(3,4-Dichloroisothiazol-5-yl)-4-(trifluoromethyl)-4,5-dihydrothiazol-4-yl-3-methylbenzoate

The title compound diethyl 2-(3,4-dichloroisothiazol-5-yl)-4-(trifluoromethyl)-4,5-dihydrothiazol-4-yl-3-methylbenzoate(C15H9Cl2F3N2O2S2, Mr = 441.26) was prepared from methyl 3,4-dichloroisothiazole-5-carboxylate as the starting material by four steps of reaction. Its structure was characterized by IR, 1H-NMR, 13C-NMR, EA and single-crystal X-ray diffraction. The crystal of the title compound belongs to the monoclinic system, space group P21/c with a = 8.8437(18), b = 16.128(3), c = 12.305(3), β = 91.68(3)o, V = 1754.4(6) 3, Z = 4, Dc = 1.671 g/cm3, μ(Mo Ka) = 0.71073 mm-1, F(000) = 888, R = 0.0384 and w R = 0.0778. Weak π-π interactions occur between the isothiazole rings and phenyl rings of adjacent molecules to form a one-dimensional chain and stabilize the crystal structure. Bioassay indicates that the title compound has good activity against the fungi and TMV tested.