4-氯乙酰乙酸乙酯的连续合成工艺研究

doi:10.16597/j.cnki.issn.1002-154x.2025.05.006

4-氯乙酰乙酸乙酯的连续合成工艺研究

沈介发* 陈代祥 马晓明 辜顺林
(常州大学 药学院 生物与食品工程学院，常州 213164)

摘 要 以双乙烯酮和氯气为原料，二氯甲烷为溶剂，采用微通道反应器进行连续氯化反应合成 4-氯乙酰乙酸乙酯，考察不同反应条件对其产率的影响。结果表明，在 20% (质量分数)的双乙烯酮-二氯甲烷溶液中，氯气与双乙烯酮物质的量比为 1.1 : 1，反应温度为 -10 ℃，氯气与双乙烯酮溶液总流速为 60 mL·min${}^{-1}$−1，停留时间为 1 min 的条件下，双乙烯酮氯化反应合成 4-氯乙酰乙酸乙酯具有较高的收率，达到 93.7%，产品提纯后含量达 98.6%。

关键词 4-氯乙酰乙酸乙酯 双乙烯酮 微通道反应 氯化

Study on the Continuous Synthesis of Ethyl 4-Chloroacetate

SHEN Jiefa* CHEN Daixiang MA Xiaoming GU Shunlin
(School of Pharmacy & School of Biological and Food Engineering, Changzhou University, Changzhou 213164, China)

Abstract Continuous chlorination in a microchannel reactor was used to improve the yield of ethyl 4-chloroacetoacetate, which was using diketene and chlorine gas as raw materials, dichloromethane as solvent, and the effect of different reaction condition was also investigated. The results showed that 4-ethyl chloroacetoacetate was prepared in dichloromethane solvent with the concentration of 20% (mass fraction), the molar ratio of chlorine gas to diketene was 1.1 : 1, the reaction temperature was -10 ℃, the total flow rate of chlorine gas and diketene solution was 60 mL·min${}^{-1}$−1, and the residence time was 1 minute. The yield of the product reached 93.7%, and the content of the product after purification reached 98.6%. It could be seen from the above that continuous chlorination by microchannel reactor could improve the product yield.

Keywords 4-ethyl chloroacetate diketene microchannel reaction chlorination