Abstract: Diethyl thiodiglycolate was efficiently synthesized via the nucleophilic substitution of ethyl chloroacetate with Na2S•3H2O. The effects of molar ratio of Na2S•3H2O to ethyl chloroacetate，solvent and reaction temperature on the reaction rate and product yield were investigated. The maximum yield of diethyl thiodiglycolate reached 81.3% with a purity of 99% when the reaction was carried out with a molar ratio of Na2S•3H2O to ethyl chloroacetate of 0.75∶1 in 250 mL cyclohexane under reflux at 81 ℃ for 4 h. And the recovery rate of cyclohexane is more than 80%.

Key words: ethyl chloroacetate, Na₂S?3H₂O, diethyl thiodiglycolate, synthesis technology

摘要： 以氯乙酸乙酯和硫化钠（Na₂S?3H₂O）为原料，通过亲核取代反应制备硫代二甘酸二乙酯。重点研究了溶剂体系、物料比、反应温度等反应条件对反应速率及产物收率的影响。在溶剂环己烷用量250 mL，硫化钠（Na₂S?3H₂O）与氯乙酸乙酯的摩尔比为0.75∶1，反应温度81 ℃，反应时间4 h的反应条件下，硫代二甘酸二乙酯的收率达81.3%，纯度在99%以上。溶剂环己烷回收率80%以上。

关键词: 氯乙酸乙酯, 硫化钠, 硫代二甘酸二乙酯, 合成工艺