摘要
以80%水合肼与37%浓盐酸为起始原料得到二盐酸肼,然后在水中与二氰二胺缩合环化合成了标题化合物,收率89%,精制后纯度达到99%以上,m.p.208～210℃。合成的最佳反应条件为：温度48～50℃,反应时间2 h,二氰二胺与二盐酸肼最佳料比为1∶1.1,pH控制在10.4～10.8。并利用元素分析、红外光谱、核磁共振光谱、质谱等分析手段对其结构进行了表征。
Hydrazine dihydrochloride was obtained from the reaction of 80% hydrazine hydrate with 37% hydrochloric acid.3,5-Diamino-1,2,4-triazole（DAT） was synthesized by condensation of hydrazine dihydrochloride with cyanoguanidine followed by cyclization with the product yield reaching 89%.The purity of refined product was over 99% and its melting point was 208～210 ℃.Its structure was characterized by IR,NMR,MS and elemental analysis.The reaction conditions were optimized,and the optimal reaction conditions specified a reaction temperature of 48～50 ℃,a reaction time of 2 h,a ratio between cyanoguanidine：hydrazine（mol）=1∶1.1,and a pH value of 10.4～10.8.
出处
《化学试剂》
CAS
CSCD
北大核心
2007年第9期563-565,共3页
Chemical Reagents
基金
"十一五"兵器预研支撑基金项目(40406020302)
