肼基甲酸叔丁酯的合成工艺

化工进展

肼基甲酸叔丁酯的合成工艺

徐东超1，曲敏杰1，李成斌2，姜殿平2，阮久勇1，刘艳喜1

1大连工业大学，辽宁大连 116034；2大连奇凯医药科技有限公司，辽宁大连 123000

出版日期:2011-11-05 发布日期:2011-11-05

Study on t-butyl carbazate synthesis

XU Dongchao1，QU Minjie1，LI Chengbin2，JIANG Dianpin2，RUAN Jiuyong1，LIU Yanxi1

1Dalian Polytechnic University，Dalian 116034，Liaoning，China；2Dalian Qi-Chem Pharmaceutical Technology Company Limited，Dalian 12300，Liaoning，China

Online:2011-11-05 Published:2011-11-05

摘要/Abstract

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。

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 .

徐东超1，曲敏杰1，李成斌2，姜殿平2，阮久勇1，刘艳喜1. 肼基甲酸叔丁酯的合成工艺[J]. 化工进展.

XU Dongchao1，QU Minjie1，LI Chengbin2，JIANG Dianpin2，RUAN Jiuyong1，LIU Yanxi1. Study on t-butyl carbazate synthesis[J]. Chemical Industry and Engineering Progree.