2,5-二乙氧甲酰氨基-1,3,4-噻二唑超分子化合物的合成和晶体结构  

Synthesis and Crystal Structure of Supramolecular Compound 2,5-Bis-(ethoxycarbonylamino)-1,3,4-thiadiazole

作　　者：林奇[1] 张有明[1] 魏太保[1] 高黎明[1] 

机构地区：[1]西北师范大学化学化工学院甘肃省高分子材料重点实验室,兰州730070

出　　处：《有机化学》2005年第3期290-294,共5页Chinese Journal of Organic Chemistry

基　　金：国家自然科学基金(No.20371040);甘肃省教育科研基金(No.021-23);西北师范大学知识与科技创新工程资金(No.02-18)资助项目.

摘　　要：报道了一种用1,6-二取代二硫脲在DMF中加热回流直接脱H2S关环合成2,5-二取代1,3,4-噻二唑类化合物的新方法,并用此方法合成了2,5-二乙氧甲酰氨基-1,3,4-噻二唑.用元素分析、核磁共振氢谱、红外光谱进行了表征,用X射线单晶衍射法确定了其单晶结构.晶体属单斜晶系,P21/c空间群,a=1.0093(4)nm,b=0.9035(4)nm,c=1.2924(6)nm,β=96.785(9)°,V=1.1703(9)nm3,Z=4,Dc=1.477g/cm3,F(000)=544,μ=0.287mm-1.该化合物通过分子间氢键形成了一种二维网状结构的超分子,由于分子间的作用力使其分子又沿c轴呈层状堆积.A novel method for the synthesis 2,5-bis-substituted-1,3,4-thiadiazoles by direct cyclization of 1,6-bis-substituted dithiourea in refluxing DMF solution is presented. Supramolecular compound 2,5-bis(ethoxycarbonylamino)-1,3,4-thiadiazole was synthesized via this method, and the structure was determined by elemental analysis, IR, H-1 NMR and X-ray diffraction analysis. Crystal data: monoclinic, space group 3 P2(1)/c, a=1.0093(4) nm, b=0.9035(4) nm, c=1.2924(6) nm, beta=96.785(9)degrees, V=1.1703(9) nm(3) Z=4, D-c = 1.477 g/cm(3), F(000) = 544,,mu = 0.287 mm(-1). The supramolecule with two-dimensional netlike structure is formed by intermolecular hydrogen bonding.

关 键 词：超分子化合物 X射线单晶衍射 二维网状结构 氨基 单斜晶系 晶体结构 1 3 4-噻二唑 合成 取代 环合 

分 类 号：TQ455[化学工程—农药化工]