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

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, D_c＝1.477 g/cm³, F(000)＝544, μ＝0.287 mm^－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.

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

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, ¹H NMR and X-ray diffraction analysis. Crystal data: monoclinic, space group P2₁/c, 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, D_c＝1.477 g/cm³, F(000)＝544, μ＝0.287 mm^－1. The su-pramolecule with two-dimensional netlike structure is formed by intermolecular hydrogen bonding.