摘要
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.
作者
刘菲
赵胜勇
王芳
张晨
刘海彪
LIU Fei1,2,3, ZHAO Shengyong1,2, WANG Fang1, ZHANG Chen1, LIU Haibiao1,2(1. Henan Chemical Industry Research Institute Co. Ltd., Zhengzhou 450052, China; 2. Adsorption and Separation of Industrial Wastewater Engineering Technology Research Center of Henan Province, Zhengzhou 450052, China; 3. Henan Academy of Quality Inspection and Test Center, Zhengzhou 450002, China)
出处
《河南科学》
2018年第9期1357-1361,共5页
Henan Science
基金
河南省科学院质量检验与分析测试中心基本科研项目(18Jk16001)