摘要
目的:在制备DM1的过程中研究DM1的聚合物杂质聚合物1的简便合成方法,以期在DM1制备过程中有效控制该杂质的产生。方法:DM1在1,3-二甲基-2-咪唑啉酮中很容易脱氢聚合,生成聚合物1。结果:所得聚合物1的化学结构已经得到质谱、核磁共振氢谱、核磁共振碳谱等检测的确证。结论:本合成方法操作简便,不需繁琐的后处理或柱层析纯化即能获得高纯度的聚合物1,可直接用作DM1有关物质质量控制的对照品。
Objective:To synthesize DM1 and study a simple method for the synthesis of dimer 1 impurity,so as to effectively control the production of this impurity in the preparation of DM1.Methods:DM1 could be easily dehydrogenated and polymerized in 1,3-dimethyl-2-imidazolidinone to form dimer 1.Results:The chemical structure of the obtained dimer 1 was confirmed by MS,1 H-NMR,13C-NMR.Conclusion:This synthetic method is simple and can obtain high purity dimer 1 without the purification of complicated post-treatment or column chromatography.It can be directly used as reference for quality control of DM1 related substances.
作者
朱阳
姚长亮
夏广兵
ZHU Yang;YAO Changliang;XIA Guangbing(Central Research Institute of Shanghai Pharmaceutical Group Co.,Ltd.,Shanghai 201203,China)
出处
《上海医药》
CAS
2022年第23期75-78,共4页
Shanghai Medical & Pharmaceutical Journal
