摘要
以(2S)-1-(3-巯基-2-甲基-1-氧代丙基)-L-脯氨酸为起始物料,经水解、盐析、精制合成了卡托普利,总收率85%,纯度99.72%,单杂小于0.1%。基于该工艺合成了卡托普利的5种杂质,纯度均大于95.0%,结构经1H NMR,13C NMR和HR-MS(ESI)确证。
Captopril was synthesized by hydrolysis of(2S)-1-(3-acetylthio-2-methyl-1-oxopropyl)-L-proline with diluted hydrochloric acid,the yield was 85%,and the purity of Captopril was 99.62%,while all the impurities were below 0.1%.Five related impurities were synthesized based on this process,and the structures were confirmed by 1H NMR,13C NMR and HR-MS(ESI).
作者
孙忠华
叶欣
王吉
胡小丽
陈益林
宦玉亮
朱怡君
SUN Zhong-hua;YE Xin;WANG Ji;HU Xiao-li;CHEN Yi-lin;HUAN Yu-liang;ZHU Yi-jun(Changzhou Pharmaceutical Factory Co.,Ltd.,Shanghai Pharma,Changzhou 213000,China)
出处
《合成化学》
CAS
北大核心
2020年第4期314-318,共5页
Chinese Journal of Synthetic Chemistry
基金
江苏省博士后基金资助项目(2018K264C)
2018年度江苏省“双创人才”计划。
关键词
卡托普利
水解
工艺改进
杂质合成
脯氨酸
Captopril
acid hydrolysis
process improvement
impurity synthesis
proline
