摘要
以D-酒石酸为拆分试剂,采用程序降温结晶法,对外消旋α-苯乙胺的拆分工艺进行了探究。通过对结晶的工艺、溶剂、温度等条件的优化试验,确定了外消旋α-苯乙胺的最佳拆分工艺,其中(R)-(+)-α-苯乙铵.D-酒石酸盐晶体收率高达95.0%,水解、精馏得(R)-(+)-α-苯乙胺,收率86.5%,ee值为93.0%,[α]2D0+38.3°。同时,开发了一种在四氢呋喃溶液中硫酸酸化D-酒石酸钠回收D-酒石酸的新方法,D-酒石酸的回收率93.0%。其拆分工艺简单,生产成本低,具有良好的工业应用价值。
Using D -tartaric acid as resolving agent, with a programmed cooling crystallization, the resolution process of racemic α- phenylethylamine was studied. The resolving conditions such as the amount of solvent and crystal- lization temperature were optimized. Under the best condition, （R） - （ ＋ ） - α-phenylethylamine was obtained in 86.5% yield and 93.0% ee with [ a] 20 3o. D ＋ 38. Meanwhile a new kind of tartaric acid recovery method was also devel- oped from the solution of sodium tartrate in THF using sulfuric acid as acidifer. D - tartaric acid was recovered in 93.0% yield. The resolution process was simple, low cost and had the value of industrial applications.
出处
《广州化工》
CAS
2013年第5期5-7,共3页
GuangZhou Chemical Industry
基金
国家自然科学基金资助项目(No.21072037)
关键词
D-酒石酸
(±)-α-苯乙胺
拆分
酒石酸回收
D - tartaric acid
（ ＋ ） - α- phenylethylamine
resolution
tartaric acid recovery
