4-[1,2,4]三氮唑-1-基甲基苯腈的合成

Synthesis of 4-[1,2,4] Triazol-1-Ylmethyl-Benzonitrile

改进4-[1,2,4]三氮唑-1-基甲基苯腈的合成方法,以价廉易得的对氰基氯苄代替对氰基溴苄,研究对氰基氯苄与1H-[1,2,4]三氮唑的N-烃基化反应及合成4-[1,2,4]三氮唑-1-基甲基苯腈的工艺条件.实验所选用的最佳工艺条件:对氰基氯苄为0.03 mol,1H-[1,2,4]三氮唑用量为0.045 mol,乙腈溶剂为20 mL,混合碱(无水碳酸钾和氢氧化钾的量比为1∶1)的总用量为0.03 mol,反应温度为70℃,反应时间为5 h,在此条件下,4-[1,2,4]三氮唑-1-基甲基苯腈的收率可达76%.

Synthesis method of 4-[1, 2,4]triazol-1-ylmethyl-benzonitrile was improved by using the cheaper 4-（chtoromethyl） ben-zonitrile instead of 4-（bromomethyl） ben-zonitrile as the raw material. Reaction conditions for the preparation of 4-[1,2,4] triazol-1-ylmethyl-benzonitrile from 4- （chloromethyl） ben-zonitrile and 1 H-[ 1,2,4] triazole by N-hydrocarbylation were investigated. The experimental results indicated that the optimal reaction conditions are as follow： 4-（chloromethyl） ben-zonitrile 0.03 mol, 1 H-[1,2,4] triazole 0. 045 mol, acetonitrile solvent 20 mL, the mixed base （anhydrousK2CO3 ： KOH=1： 1） 0.03 mol, temperature 70 ℃ and reaction time 5 h; under this reaction condition, the yield of the objective compound can reach 76%.