摘要
三步法合成醋酸卡泊芬净粗品的限速步骤是第二步还原反应,该步反应的转化率与中间体D1的质量密切相关。对醋酸卡泊芬净中间体D1的结晶工艺进行了优化,最优工艺如下:D1∶甲醇∶乙酸乙酯=1∶6∶24(g∶mL∶mL),20℃下将乙酸乙酯滴加至D1的甲醇溶液中,控制乙酸乙酯在1h内滴完,养晶1h。此条件下,中间体D1的收率、纯度和含量分别达到92.4%、92.7%和89.4%,提高了后处理操作的便捷性,显著提高了第二步还原反应的转化率,具有较强的实际意义。
The second-step reduction reaction is the rate-limiting step of three-step synthesis of crude Caspofungin acetate,the conversion rate of the second-step reduction reaction is closely related to the quality of intermediate D1.We optimized crystallization process of Caspofungin acetate intermediate D1.The optimum conditions are determined as follows:D1∶methanol∶ethyl acetate is 1∶6∶24(g∶mL∶mL),adding ethyl acetate into D1 methanol solution within 1 h at 20℃,and the crystal growth time is 1 h.Under above conditions,the yield,purity,and content of the intermediate D1 reach 92.4%,92.7%,and 89.4%,respectively,which improved the convenience of post-processing operation,and significantly improved the conversion rate of the second-step reduction reaction.The optimized crystallization process has strong practical significance.
作者
周陈锋
杜明镜
王宏伟
吴豪杰
ZHOU Chenfeng;DU Mingjing;WANG Hongwei;WU Haojie(Hangzhou Zhongmei Huadong Pharmaceutical Co.,Ltd.,Hangzhou 310011,China)
出处
《化学与生物工程》
CAS
2019年第8期62-64,共3页
Chemistry & Bioengineering
关键词
醋酸卡泊芬净
中间体D1
结晶工艺
转化率
Caspofungin acetate
intermediate D 1
crystallization process
conversion rate
