4-氯乙酰乙酸乙酯的连续合成工艺  

Continuous Synthesis Process of Ethyl 4-Chloroacetoacetate

作　　者：沈介发[1] 陈代祥[1] 马晓明[1] 辜顺林[1] SHEN Jiefa;CHEN Daixiang;MA Xiaoming;GU Shunin(School of Pharmacy,Changzhou Univercity,Changzhou 213164,China)

机构地区：[1]常州大学药学院,江苏常州213164

出　　处：《化工管理》2023年第36期156-161,共6页Chemical Engineering Management

摘　　要：文章采用微通道反应器进行连续氯化反应来提高4-氯乙酰乙酸乙酯的收率。将双乙烯酮和氯气分别溶解于二氯甲烷,再通过计量泵按比例泵入微通道反应器中,在正压条件下以一定反应温度、时间进行反应。其结果表明,在双乙烯酮含量为20%、氯气含量为10%、氯气与双乙烯酮摩尔比为1.05∶1.00、反应温度为-10℃、流速为60 mL/min、停留时间为1 min的反应条件下制备的4-氯乙酰乙酸乙酯产品,其产品收率达到96.7%,产品提纯后含量达到98%以上。A microchannel reactor was used for continuous chlorination to improve the yield of ethyl 4-chloroacetoacetate.In this paper,the divinyl ketone and chlorine gas were dissolved in dichloromethane,and then proportionally entered the microchannel reactor through a metering pump,and the reaction was carried out at a certain reaction temperature and time under positive pressure.The results showed that ethyl 4-chloroacetoacetate was prepared under the content conditions of divinyl ketone content of 20%,chlorine gas content of 10%,molar ratio of chlorine gas to divinyl ketone of 1.05∶1.00,reaction temperature of -10℃,flow rate of 60 mL/min and residence time of 1 min.The yield of the product reached 96.7%,and the content of the product reached more than 98% after purification.

关 键 词：4-氯乙酰乙酸乙酯 双乙烯酮 微通道反应 氯化反应 

分 类 号：TQ460[化学工程—制药化工]