3-(a-甲氧基)甲烯基苯并呋喃-2(3H)-酮的合成与优化  

Optimization for the Synthesis of 3-(a-Methoxy)methylenebenzo-furan- 2(3H)-one

作　　者：周林芳[1] 陈志荣[1] 缪程平[1] 尹红[1] 

机构地区：[1]浙江大学联合化学反应工程研究所,杭州310027

出　　处：《农药》2004年第9期414-416,共3页Agrochemicals

摘　　要：以邻氯苯乙酸为原料,经过水解、酯化、甲氧甲烯化合成3-(a-氧基)甲烯基苯并呋喃-2(3H)-酮。改进了第一步反应的后处理工艺,通过单因素实验确定水解反应催化剂的最佳用量为催化剂A(8-羟基喹啉铜) :邻氯苯乙酸=0.075:1(摩尔比),两步反应的总收率为84.05%。通过单因素实验得到甲氧甲烯化反应的较佳工艺条件为苯并呋喃-2(3H)-酮:原甲酸三甲酯:乙酸酐=1:2:4,反应温度100℃,反应时间12h,反应收率达到93.59%。The title compound was synthesized from o-chlorophenylacetic by hydrolyzation, esterificationand methoxymethlenation.The operation conditions of each step were optimized. The yield of the first andsecond reactions reaches 84.05% when the molar ratio of catalyst A to o-chlorophenylacetic equales to 0.075:1. In methoxymethlenation, 93.59% yield has been obtained when the molar ratio of benzofuran-2(3H)-one totrimethyl orthoformate to acetic anhydride is 1:2:4, at 100℃, reaction 12h.

关 键 词：邻氯苯乙酸 合成 后处理 

分 类 号：TQ453[化学工程—农药化工]