【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。加成反应的最佳工艺条件为:当DMF与溴的摩尔比为1∶1.1,在4℃下反应10h,产率约为71%。消除反应的最佳工艺条件为:反应物料摩尔比为1∶1,在60℃下反应2.5h,可得灰白色固体α-BrDMF。用红外光谱和质谱对产物结构进行了表征。皮肤过敏性测试表明α-BrDMF无明显致敏性。更多还原

【Abstract】 The process of synthesizing α-bromo dimethyl fumarate(α-BrDMF) includes two reactions: Bromine electrophilic added to dimethyl fumarate(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 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 hours, the yield could reach 71%. The optimum reaction conditions of the elimination reaction is when DBDMF and sodium hydroxide(molar ratio 1∶1) reacted at 60 ℃ for 2.5 hours, then α-BrDMF was formed as a off-white crystal. The molecular structure of product was characterized and confirmed by infra-red spectrum and mass spectrum. Skin tests showed that α-BrDMF do not stimulate to skin.更多还原