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作 者:廖喜慧[1] 刘于民[1] 沈玉堂[1] 王爱丽[1] 殷恒波[1]
出 处:《化工进展》2012年第3期654-657,共4页Chemical Industry and Engineering Progress
基 金:江苏省研究生创新基金项目(CX10B-259Z)
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。Diethyl thiodiglycolate was efficiently synthesized via the nucleophilic substitution of ethyl chloroacetate with Na2S'3H20. The effects of molar ratio of Na2S-3H20 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'3H20 to ethyl chloroacetate of 0.75 : 1 in 250 mL cyclohexane under reflux at 81 ~C for 4 h. And the recovery rate of cyclohexane is more than 80%.
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