邻苯二甲酰亚胺类肼解反应改进  

Improvement of Hydrazinolysis Reactions of Phthalimides

作　　者：汪洪玲 万聪聪 段吉婷 郭斗 张翔 WANG Hongling;WAN Congcong;DUAN Jiting;GUO Dou;ZHANG Xiang(College of Chemistry&Pharmacy,Northwest A&F University,Yangling 712100,China)

机构地区：[1]西北农林科技大学化学与药学院,陕西杨凌712100

出　　处：《合成化学》2023年第11期889-894,共6页Chinese Journal of Synthetic Chemistry

基　　金：陕西省青年基金资助项目(2022JQ-144)。

摘　　要：邻苯二甲酰亚胺类化合物在肼解过程中会生成伯胺和邻苯二甲酰肼。在纯化过程中,邻苯二甲酰肼往往需要进行反复结晶、多次过滤及柱色谱等繁琐的操作去除。本文以氢氧化钠水溶液处理肼解后的反应液,可将邻苯二甲酰肼成盐后溶于水中,而伯胺产物通过简单的萃取得以分离,收率可达90%以上。改进后的方法简单快捷,无需柱纯化,适合大规模生产,为多数苄基、烷基及芳基型伯胺的合成及纯化提供了新的思路。Hydrazinolysis of phthalimides will generate primary amine and phthalhydrazide.The removal of phthalhydrazide generally requires tedious operations such as repeated crystallization,multiple filtration and column chromatography during the purification process.In this protocol,the resulting mixture after hydrazinolysis is treated with sodium hydroxide aqueous solution till the salification of phthalhydrazide.Then the mixture is directly extracted to yield more than 90%of the primary amine.The improved operation is simple and fast without column purification,and suitable for extensive production,providing a new idea for the synthesis and purification of most benzyl,alkyl and aryl primary amines.

关 键 词：Gabriel合成法 肼解反应 邻苯二甲酰亚胺 邻苯二甲酰肼 氢氧化钠 萃取 伯胺 

分 类 号：O622.6[理学—有机化学]