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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。
Synthesis of α-Bromofuranic acid dimethyl ester (α-BrDMF) is divided into two steps: with glacial acetic acid as a solvent, dimethyl fumarate (DMF) and bromine electrophilic reaction to form fumaric acid bis Methyl ester dibromide (d-BrDMF); d-BrDMF and ethanol solution of sodium hydroxide were heated to eliminate the reaction available α-BrDMF. The optimum conditions for the addition reaction were as follows: when the molar ratio of DMF to bromine was 1: 1.1, and reacted at 4 ℃ for 10h, the yield was about 71%. The best reaction conditions were as follows: the molar ratio of reactants was 1: 1, reacted at 60 ℃ for 2.5h to obtain α-BrDMF as an off-white solid. The product structure was characterized by IR and MS. Skin allergy tests showed that alpha-BrDMF had no significant sensitization.