L-^(10)BPA中间体合成工艺优化及连续流可行性工艺研究  

Optimization of L-^(10)BPA Intermediate Synthesis Process and Feasibility Study of Continuous Flow Process

作　　者：关东 董珍 陈凯 李国威 廖竞远 黄均荣 游恒志 Guan Dong;Dong Zhen;Chen Kai;Li Guowei;Liao Jingyuan;Huang Junrong;You Hengzhi(Shenzhen Zhonghe Headway Bio-Sci&Tech Co.,Ltd.,Guangdong,518057;Harbin Institute of Technology(Shenzhen),Guangdong,518055)

机构地区：[1]深圳市中核海得威生物科技有限公司,广东518057 [2]哈尔滨工业大学(深圳),广东518055

出　　处：《当代化工研究》2023年第21期143-145,共3页Modern Chemical Research

摘　　要：利用硼-10酸作为原料与正丁醇反应后,再与格氏试剂异丙基氯化镁制备(S)-Boc-4-二羟基硼10基-苯丙氨酸。通过设计正交实验优化了该反应的釜式反应条件和后处理方式,釜式克级反应分离收率可达63%。在最优的釜式反应条件基础上进行连续流反应,制备含10B的L-10BPA中间体,反应时间由釜式反应的17h缩短至2h,分离收率达到了57%,验证了含10B的L-10BPA中间体连续流反应的可行性,且连续流工艺具有反应速度快、安全性好等优点,适合工业放大生产。After reacting with n-butanol using boron-10 acid as raw material,(S)-Boc-4-dihydroxyboron-10-phenylalanine was prepared with Grignard reagent isopropyl magnesium chloride.By designing orthogonal experiments,the tank reaction conditions and post-treatment methods of the reaction were optimized,and the separation yield of the kettle gram reaction could reach 63%.Based on the optimal tank reaction conditions,the continuous flow reaction was carried out,and the L-10BPA intermediate was prepared,and the reaction time was shortened from 17 hours to 2 hours of the kettle reaction,and the separation yield reached 57%,which verified the feasibility of the continuous flow reaction of L-10BPA intermediate,and the continuous flow process has the advantages of fast reaction speed and good safety,which is suitable for industrial scale-up production.

关 键 词：L-10BPA 连续流 工艺研究 

分 类 号：TQ253.2[化学工程—有机化工]