摘要
目的:探讨合成α-氯(2-氯)苯乙酸甲酯的工艺优化。方法:以邻氯扁桃酸甲酯为原料、二氯亚砜为氯化试剂合成α-氯(2-氯)苯乙酸甲酯;设计正交试验,以邻氯扁桃酸甲酯与二氯亚砜投料比、反应温度、反应时间为因素,以产率为指标优化合成工艺条件,并进行验证试验。结果:确定了最佳反应条件即邻氯扁桃酸甲酯与二氯亚砜投料比为2∶3,反应时间为1h,反应温度40℃;以此条件合成产品收率≥92%,纯度≥99%。结论:所得合成工艺条件适用于合成α-氯(2-氯)苯乙酸甲酯。
OBJECTIVE：To approach the optimization of synthetic process of α-chloro-o-chlorophenyl acetate.METHODS：α-chloro-o-chlorophenylacetate was synthesized with o-chlorophenylacetic acid and thionyl chloride.The synthetic process of α-chloro-o-chlorophenylacetate was optimized by orthogonal test with the ratio of raw materials,reaction temperature,reaction time as factors and with production efficiency as index.And the results of study were verified.RESULTS：The optimal synthesis conditions were as follows：ratio of o-chlorophenylacetic acid to thionyl chloride was equal to 2：3;the reaction time and temperature were 1 h and 40 ℃,respectively.The yield was more than 92% and purity of production was more than 99%.CONCLUSION：Established synthetic process is suitable for the synthesis of α-chloro-o-chlorophenylacetate.
出处
《中国药房》
CAS
CSCD
北大核心
2010年第25期2350-2352,共3页
China Pharmacy
基金
重庆莱美药业股份有限公司对本课题的资助
