摘要
以甲酰胺和水合肼为原料合成1,2,4-三氮唑,选定反应时间、反应温度和物料比作为反应控制条件,进行正交及优化实验,得出最优合成条件为n（甲酰胺）∶n（水合肼）=1∶2.0,反应温度175~180℃,反应时间50 min,在此条件下1,2,4-三氮唑粗产物收率为88.6%,并测定熔点。粗产物经乙醇重结晶后用红外光谱（IR）、核磁共振氢谱（1H NMR）进一步验证其结构。
1,2,4-triazole was synthesized from formamide and hydrazine hydrate as raw materials.The orthogonal experiments were put forward by discussing and comparing some reaction conditions such as time,temperature and materials＇ ratios.Optimal conditions：n（formamide）：n（hydrazine hydrate） = 1∶2.0,reaction temperature 175～180℃,reaction time 50 min,yield of raw 1,2,4-triazole is 88.6%.The Melting point of crude product is determined and the products was further recrystallized from ethanol.The structure of the final product was confirmed by IR,1H NMR spectra.
出处
《天津化工》
CAS
2012年第2期20-22,共3页
Tianjin Chemical Industry
关键词
甲酰胺
水合肼
1
2
4-三氮唑
合成
formamide
hydrazine hydrate
1
2
4-triazole
synthesis
