摘要
以4-氯乙酰乙酸乙酯(Ⅰ)和甘氨酰胺盐酸盐(Ⅱ)为原料,经"一锅法"反应得到奥拉西坦关键中间体2,4-二氧代吡咯烷-1-基乙酰胺。经过碱、溶剂、温度、反应物配比的筛选,确定较佳的合成工艺条件为n(Ⅰ)∶n(Ⅱ)∶n(K2CO3)=1∶1.2∶2.4,乙醇作为溶剂,回流温度下滴加化合物Ⅰ,滴完后回流反应5 h,收率为78%。
(2,4-Dioxopyrrolidin-1-yl)acetamide,a key intermediate of Oxiracetam,was synthesized from ethyl 4-chloroacetoacetate( I) and glycinamide hydrochloride( II) via a one-pot reaction. The reaction conditions were optimized from base,solvent,temperature and the reactant ratio. It was found that the optimal yield 78% was obtained when compound I was added dropwisely into the solution of compound II(1.2 equiv.) and K2CO3(1.2 equiv.) in Et OH at refluxing temperature and the reactant mixture was refluxed for 5 h.
作者
童永正
顾凯
高建荣
TONG Yong-zheng GU Kai GAO Jian-rong(College of Chemical Engineering, Zhejiang University of Technology, Hangzhou , Zhejiang 310014, China)
出处
《浙江化工》
CAS
2017年第9期20-23,共4页
Zhejiang Chemical Industry