摘要
邻氯扁桃酸甲酯是合成手性药物氯吡格雷的重要中间体之一.其传统制备工艺是以邻氯扁桃酸为起始原料在硫酸及回流温度条件下经酯化反应制得.研究以相对温和的硼酸作为催化剂在常温条件下催化邻氯扁桃酸与甲醇进行的酯化反应.采用FT-IR、1H NMR、13C NMR及HRMS对产物结构进行鉴定.探讨催化剂用量、投料比、温度、反应时间对反应的影响.并针对该反应的特点对反应装置进行改进,实现连续化制备邻氯扁桃酸甲酯.
Abstract
Methyl o-chloromandelic is an important intermediate for the synthesis of clopidogrel,which is ob-tained by esterification reaction under the conditions of sulfuric acid and reflux temperature using o-chloroman-delic acid as the starting material.In this paper,relatively mild boric acid was used as a catalyst to catalyze the es-terification of o-chloromandelic acid and methanol at room temperature.The product was confirmed by FT-IR,1H NMR,13C NMR and HRMS spectra.The effects of catalyst dosage,feed ratio,temperature,and reaction time on the reaction were explored.According to the characteristics of the reaction,the reaction device is im-proved to achieve continuous preparation process for methyl o-chloromandelate.
基金项目
肇庆学院大学生创新创业训练计划项目(X202310580140)
维普
万方数据