以2,5-二巯基-1,3,4-噻二唑为原料,与水合肼缩合,生成2,5-二肼基-1,3,4-噻二唑.2,5-二肼基-1,3,4-噻二唑与苯甲酰氯反应生成2,5-二酰肼基-1,3,4-噻二唑,以POCl3为环合剂环合酰肼基-1,3,4-噻二唑,合成3,6-二取代苯基-二-1,2,4-三唑并[3,4-b]-1,3,4-噻二唑衍生物,合成的新化合物的结构通过元素分析、红外光谱、核磁共振氢谱和质谱予以证实,并提出了环化反应机理. 2,5-dimercapto-1,3,4-thiadiazole as raw materials, and hydrazine hydrate condensation, 2,5-dihydrazino-1,3,4-thiadiazole 2,5-dihydrazide 1,3,4-thiadiazole and benzoyl chloride react to form 2,5-dihydrazide-1,3,4-thiadiazole, POCl3 as cyclizing agent hydrazide-1,3 , 4-thiadiazoles, synthetic 3,6-disubstituted phenyl-di-1,2,4-triazolo [3,4-b] -1,3,4-thiadiazole derivatives, The structure of the new compounds was confirmed by elemental analysis, IR, 1H-NMR and MS, and the cyclization reaction mechanism was proposed.