Gabriel合成法制备4-氨基丁醇

Preparation of 4-Aminobutan-1-ol by Gabriel Synthesis Method

采用Gabriel合成法,首次使用4-氯丁醇、邻苯二甲酰亚胺作为初始原料,四丁基溴化铵作为相转移催化剂,反应制备N-(4-羟基丁基)邻苯二甲酰亚胺(中间体),中间体在氢氧化钠的作用下水解得到4-氨基丁醇.通过高分辨质谱、核磁共振光谱等对中间体和产品进行了表征.考察了反应溶剂、4-氯丁醇与邻苯二甲酰亚胺物质的量比、反应温度、反应时间对中间体收率的影响,优化反应条件之后4-氨基丁醇最佳的总收率为77.1%.此工艺路线具有合成方法简便、反应条件温和、产品收率高等优点,可以进行工业放大.

In the paper,the N-（4-hydroxybutyl）o-benzenedicarboximide（intermediate）was synthesized from 4-chloro-1-butanol. We took the phthalimide as the initial raw materials,tetrabutylammonium bromide as thephase transfer catalyst,gabriel as the synthesis method,and the intermediate was hydrolyzed to 4-aminobutan-1-olby sodium hydroxide. The intermediate and product structure were characterized by HRMS and 1H NMR. Theinfluences of reaction solvent,molar ratio phthalimide and 4-chloro-1-butanol,reaction temperature,reactiontime on the yield of intermediate were investigated. The total yield of 4-amino butanol was 77.1%. This new processhad many advantages,such as the simple process,mild reaction condition,high yield and could be potentially utilizedin industrial amplification.