含葑基的缩氨基硫脲、噻二唑的合成、表征与晶体结构

以(－)-葑酮为原料经中间体葑胺合成4-葑基氨基硫脲(4), 4与醛缩合得到11个未见文献报道的葑基缩氨基硫脲(5), 5用六氰合铁(III)酸钾氧化成环得到相应的2,5-二取代-1,3,4-噻二唑类化合物(6); 产物的结构经IR, NMR和元素分析确认, 并用X射线衍射法测定化合物6d的晶体结构. 化合物6d属单斜晶系, P2(1)空间群, 晶胞参数 a＝1.18719(10) nm, b＝1.48814(18) nm, c＝1.21629(12) nm, β＝118.113(2)°, Mr＝343.48, V＝1.8953(3) nm3, Dc＝1.204 Mg/m3, Z＝4, λ＝0.071073 nm, μ(Mo Kα)＝0.181 mm－1, F(000)＝736.     

含脱羧脱氢松香基的1,2,4-三唑并[3,4-b]-1,3,4-噻二唑衍生物的合成、表征及抑菌活性

用POCl3为催化剂和脱水剂,3-取代-4-氨基-5-巯基-1,2,4-三唑4和10分别与脱氢松香酸1反应制得14种未见文献报道的3-取代-6-(4′-脱羧脱氢松香基)-1,2,4-三唑并[3,4-b-]-1,3,4-噻二唑衍生物]5a~5e和11a~11i;所有化合物的结构均经IR、¹H NMR、¹³C NMR 和MS测试技术分析确认。 抑菌活性测试表明,目标化合物对白色念珠菌(C.Albicans)、大肠杆菌(E.Coli)、藤黄微球菌(M.Luteus)和痢疾志贺杆菌(S.Dysenteriae)均有一定的抑制作用。     

Synthesis,Characterization and Crystal Structure of 3-o-Fluorophenyl-6-（4-decarboxydehydroabietyl）-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole

Three novel 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles were designed,synthesized and characterized by IR,NMR and APCI-MS.3-o-Fluorophenyl-6-(4-decarboxydehydroabietyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole(6a,C28H31FN4S) was structurally determined by single-crystal X-ray diffraction.The crystal belongs to the orthorhombic system,space group P212121 with a=6.0153(14),b=12.2577(19),c=34.055(3),V=2511.0(7)3,Z=4,Mr=474.63,Dc=1.255Mg/m3,λ=0.71073 ,μ(MoKα)=0.160 mm-1,F(000)=1008,the final R=0.0555 and wR=0.1248 for 3094 observed reflections with I2σ(I).There are six rings in the crystal structure of the title compound.The dihedral angle between 1,2,4-triazole and 1,3,4-thiadiaole rings is 1.4o,and that between 1,2,4-triazole and benzene ring D 25.5o.