α-溴代富马酸二甲酯的合成  

Synthesis of α-Bromo Dimethyl Fumarate

作　　者：黄艳仙[1] 曾霞[1] 周如金[1] 

机构地区：[1]茂名学院化学与生命科学学院,广东茂名525000

出　　处：《茂名学院学报》2009年第3期1-4,共4页Journal of Maoming College

基　　金：广东省自然科学基金项目(5300953)

摘　　要：α-溴代富马酸二甲酯(α-BrDMF)的合成分为两步:以冰乙酸为溶剂,富马酸二甲酯(DMF)与溴发生亲电加成反应生成富马酸二甲酯二溴化物(d-BrDMF);d-BrDMF与氢氧化钠的乙醇溶液共热,发生消除反应可得α-BrDMF。在单因素实验的基础上通过正交实验对反应条件进行了优化,得到最佳反应条件。加成反应最佳工艺条件为:当DMF与溴的摩尔比为1:1.1,在4℃下反应10 h,产率为70.6%。消除反应最佳工艺条件为:反应物料摩尔比为1:1,在60℃下反应2.5 h,可得灰白色固体α-BrDMF。皮肤过敏性测试表明α-BrDMF无明显致敏性。The process of synthesizing α- bromo dimethyl fumarate （α- BrDMF） includes two reactions： Bromine electrophilic added to dimethyl fumaratc（DMF） in acetic acid solution forming dibromo - dimethyl fumarate （d- BrDMF）. Then d- BrDMF changed to α- BrDMF through elimination reaction in the medium of ethanol with sodium hydroxide. The technological process and conditions for preparation of α- BrDMF were optimized by single factor and orthogonal experiments. The results showed that the optimum reaction conditions of the addition reaction is when DMF and bromine （molar ratio 1：1.1） reacted at 4℃ for 10 hour, the yield could reach 70.6 %. The optimum reaction conditions of the elimination reaction is when d - BrDMF and sodium hydroxide （molar ratio 1 ： 1 ） reacted at 60℃ for 2.5 hour, then α- BrDMF was formed as a off- white crystal. Skin tests showed that α- BrDMF do not stimulate to skin.

关 键 词：防腐剂 α-溴代富马酸二甲酯 合成 

分 类 号：TQ423.96[化学工程]