Abstract:

t-butyl carbazate was synthesized by esterification of tert-butatol and hydrazinolysis of hydrazine hydrate with phenyl chloroformate as raw material. Factors in the process of esterification and hydrazinolysis were investigated. The results showed that the yield of t-butyl phenyl carbonate is about 77% when esterification reaction time is 3 h and the reaction temperature is 25～30 ℃；the yield of t-butyl carbazate is up to 93% when the mole ratio of hydrazine hydrate to t-butyl phenyl carbonate is 2∶1，the reaction temperature is 100 ℃. The overall yield is about 71.7%. The product structure was confirmed by MS and IR .

摘要：

以氯甲酸苯酯为原料，经过叔丁醇酯化、水合肼肼化得到肼基甲酸叔丁酯，考察了酯化和肼化过程中影响反应的因素。结果表明：酯化反应时间为3 h、反应温度为25～30 ℃条件下，可以得到收率为77%的叔丁基苯基碳酸酯；当水合肼与叔丁基苯基碳酸酯的摩尔比为2∶1，反应温度为100 ℃时，反应产物肼基甲酸叔丁酯的收率可以达到93%，两步总收率为71.7%，其结构经质谱和红外分析确认。