摘要
以廉价易得的二苯甲醇为起始物料,依次经氯化、氨解、酰胺化3步反应合成了(2S)-N-二苯甲基-2-吡咯甲酰胺。优化的工艺条件为:氯化反应以氯化亚砜作氯源;氨解反应纯化溶剂n(乙酸乙酯)∶n(异丙醇)=1∶3、打浆温度10~20℃;酰胺化反应时间3 h。优化后的反应总收率65.3%,产品纯度98.5%。合成路线简便,工艺稳定。
The pharmaceutical intermediate,(2S)-N-diphenylmethyl-2-pyrrolidinecarboxamide,was synthesized through a series of reactions including chlorination,ammonolysis,and amidation with using commercialized diphenylmethanol as the starting material.The main factors influencing the reactions were investigated.The experimental results showed that:using thionyl chloride as chlorine source,the solvent molar ratio of ethyl acetate to isopropyl alcohol is 1∶3,and the purification temperature is 10~20℃,the amidation time is 3 h.The overall yield amounts to 65.3%and the purity reached 98.5%.The route has mild reaction conditions and simple operation,and is suitable for industrial scale production.
作者
邓护军
王军绪
付国兵
张宁
梁春梅
DENG Hu-jun;WANG Jun-xu;FU Guo-bing;ZHANG Ning;LIANG Chun-mei(Xi'an WanLong Pharmaceutical Co.,Ltd.,Xi'an 710119,China)
出处
《精细化工中间体》
CAS
2020年第6期41-44,共4页
Fine Chemical Intermediates
基金
陕西省自然科学基础研究计划(面上)(2018JM7046)。
