4，4′-联-1，2，4-三唑的合成、表征和晶体结构

摘要

4,4′-Bis-1,2,4-triazole(2,BTr)was synthesized from N,N-dimethylformamide azine dihyfrrochloride(1)and 4-ami-no-1,2,4-triazole in toluene as solvent. The structure of BTr was characterized by 1H NMR,IR,MS and element analysis. The single crystal of BTr was also cultivated successfully and determined by a X-ray single crystal diffractometer. The effect of reaction solvent,molar ratio,time and temperature on the yield of BTr were investigated. Results show that using toluene as reaction slov-ent,the optimal conditions of preparation are as follow:molar ratio of 1 to 4-amino-1,2,4-triazole 11. 2,time 8 h,temperature 110 ℃,the yield is 86. 4%. And the crystal of title compound is orthorhombic system,space group Pnma with crystal parameters of a=0.69712(14)nm,b=0.74045(15)nm,c=1.1156(2)nm,V=0.5759(2)nm3,Z =4,Dc =1.570 g·cm -3,F(000)=280,R1 =0. 043,ωR2 =0. 1222. The two triazole rings in BTr are vertical to each other,and that should be beneficial to the stability of the molecule due to the least steric hindrance. .%以甲苯为溶剂，N，N-双（二甲基氨基亚甲基）肼二盐酸盐）（1），与4-氨基-1，2，4-三唑缩合制得4，4′-联-1，2，4-三唑（2，BTr），产品经1 H NMR，IR，MS和元素分析确证结构，并成功培养出BTr单晶。考察了反应中溶剂、投料比、时间及温度对BTr产率的影响。结果表明，缩合反应的最佳溶剂为甲苯，最优工艺条件为 n（1）n（4-氨基-1，2，4-三唑）＝11．2，时间为8 h，温度为110℃，所得收率可达86．4％。经 X 射线单晶衍射仪测定，BTr 单晶晶体为斜方晶系，属 Pnma空间群，晶体学参数为：a＝0．69712（14）nm，b＝0．74045（15）nm，c＝1．1156（2）nm，V＝0．5759（2）nm3，Z＝4，Dc ＝1．570 g·cm -3，F（000）＝280， R1＝0．043，ωR2＝0．1222，BTr分子中两个单三唑环在空间相互垂直，该立体结构空间位阻小，利于分子稳定。