1,2,3-三氮唑的合成工艺研究

Study on Synthesis of 1,2,3-triazole. XIAO Guo-min, et al.

以对甲苯磺酰肼为原料合成 1,2 ,3 三氮唑。研究了各种工艺条件对收率的影响 ,获得了较佳合成工艺 :用苯作溶剂 ,对甲苯磺酰氯与水合肼配比为 1∶2 (mol) ,在 60～ 70℃下进行缩合反应制得对甲苯磺酰肼 ,收率为 80 6% ;对甲苯磺酰肼与乙二醛以配比 1∶2 7(mol)反应后 ,通入定量的氨气进行环合反应生成 1,2 ,3 三氮唑 ,收率达 66 8%

Some synthetic methods of 1,2,3 triazole were introduced in this article. The process of preparation from p toluene sulfonyl hydrazine was selected for its advantages.Experiments were done to compare the different conditions of reaction, and the optimal condition to synthesis of 1,2,3 triazole was obtained as follows: p toluene sulfonyl hydrazine was prepared by reaction of MeC 6H 4SO 2Cl (a) with H 2NNH 2·H 2O(b) in presence of benzene as solvent and M ratio of a∶b=1∶2 at 60～70℃. Then high purity 1,2,3 triazole was obtained by the reaction of p toluene sulfonyl hydrazide and glyoxal at M ratio 1∶2.7 followed by the treatment of the intermediate with ammonia, the yield over 66.8%.