摘要
对现有文献报道的马赛替尼合成工艺进行优化改进.以2-甲基-5-硝基苯胺为原料,经缩合、噻吩环化、还原氢化、酰化等反应制备马赛替尼,产物结构经电喷雾质谱(ESI-MS),核磁共振氢谱(~1 H-NMR),核磁共振碳谱(^(13)C-NMR)等确证,并对其中的合成条件进行优化对比研究.结果表明:优化工艺后,马赛替尼的总收率为37.3%(以2-甲基-5-硝基苯胺计),与文献报道的工艺相比,提高了9%;优化后的工艺具有反应时间短、成本低、收率高等特点,更易应用于工业化生产.
The synthesis process of masitinib which was reported in the literature was improved.Masitinib was synthesized by using 2-methyl-5-nitroaniline as a raw material,via condensation,cyclization,hydrogenation and acylation etc,its structure was confirmed by electrospray ionization mass spectrometry(ESI-MS),proton nuclear magnetic resonance(1H-NMR)and carbon 13 nuclear magnetic resonance(13 C-NMR),and the reaction conditions of some steps were optimized.The results show that the yield of masitinib after optimization was up to 37.3%(in terms of 2-methyl-5-nitroaniline),which is 9%higher than that reported in literature;the optimized process has the characteristics such as short reaction time,low cost and high yield,and it′s easier to apply to industrial production.
作者
张嘉颖
裘京晓
黄程勇
吴振
王立强
ZHANG Jiaying;QIU Jingxiao;HUANG Chengyong;WU Zhen;WANG Liqiang(School of Biomedical Sciences,Huaqiao University,Quanzhou 362021,China;Affiliated Hospital,Beijing International Studies University,Beijing 100024,China;School of Pharmaceutical Sciences,Xiamen University,Xiamen 361102,China)
出处
《华侨大学学报（自然科学版）》
CAS
北大核心
2019年第2期215-220,共6页
Journal of Huaqiao University(Natural Science)
基金
国家重点研发计划项目(2016YFE0101700)
华侨大学研究生科研创新能力培育计划资助项目(17014071021)
