4-羟基香豆素的合成新工艺

Abstract

考察以邻羟基苯乙酮与碳酸二乙酯为原料反应合成4-羟基香豆素的新方法。通过正交实验对相转移催化剂添加量、碱性缩合剂用量、加料温度、反应时间进行考察,得出此方法合成4-羟基香豆素的较优工艺条件为:原料摩尔比为n(邻羟基苯乙酮):n(碳酸二乙酯):n(甲醇钠):n(聚乙二醇-400)=1:2:3.0:0.42,在5~10℃温度下加料,120℃反应2.5 H,收率为65.7%。产物经熔点、Ir、--1HnMr、--(13)CnMr进行鉴定。

4-Hydroxycoumarin was synthesized by the reaction of 2-hydroxyacetophenone with diethyl carbonate via the catalyst of sodium methoxide and polyethylene glycol-400.According to the orthogonal design experiments about the dosages of polyethylene glycol-400,the dosages of alkali,the feed temperture and the reaction time.The optimal reaction conditions were as follows:xylene as the solvent,n(2-hydroxyacetophenone):n(diethyl carbonate):n(sodium methoxide):n(polyethylene glycol-400) = 1:2.0:3.0:0.42.Feed under the temperature of 5—10℃.The reaction mixture was heated at 120℃for 2.5 h.4-Hydroxycoumarin was produced in 65.7%yield.The product was characterized by Melting point meter,IR,--1HNMR and --(13)CNMR.