CIESC Journal

• 精细化工 • 上一篇    下一篇

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. 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:2011-11-21

Study on t-butyl carbazate synthesis

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

  1. 1Dalian Polytechnic University,Dalian 116034,Liaoning,China;2Dalian Qi-Chem Pharmaceutical Technology Company Limited,Dalian 12300,Liaoning,China
  • Online:2011-11-05 Published:2011-11-21

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2530 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21,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 2530 the yield of t-butyl carbazate is up to 93% when the mole ratio of hydrazine hydrate to t-butyl phenyl carbonate is 21the reaction temperature is 100 . The overall yield is about 71.7%. The product structure was confirmed by MS and IR .