摘要
采用市售伊马替尼中间体(N-(5-氨基-2-甲基苯基)-4-(3-吡啶基)-2-氨基嘧啶)为原料,经酰化、胺化和成盐3步制得甲磺酸伊马替尼。并针对胺化制备伊马替尼步骤中普遍存在的反应温度高、能耗大、反应收率低及后处理步骤繁琐的问题进行了工艺改进。结果表明,降低反应温度,控制了杂质的生成,同时将后处理步骤中采用的萃取、洗涤、浓缩、重结晶等操作改为析晶过滤,简化了操作过程,提高了反应收率和产品质量。
Using commercially available intermediate （ 6-methyl-N-（ 4-（ pyridin-3-yl ） pyrimidin-2-yl ） nzene-1,3- diamine） as raw material, imatinib mesylate is prepared via acylation reaction, amination reaction and salt forming reaction subsequently. The process improvement is performed to solve the problems such as high reaction temperature, large energy consumption, low yield, and so on. The results show that, the measures such as decreasing reaction temperature, controlling purity generation and replacing extraction, washing, condensation and rcerystallization steps with crystallization step, simplify the production process and improve the reaction yield and product quality.
出处
《现代化工》
CAS
CSCD
北大核心
2012年第9期47-49,共3页
Modern Chemical Industry
基金
科技部"十一五"重大新药创制(2011ZX09401-306)
国家"973"课题(2012CB724002)
关键词
伊马替尼
合成
工艺改进
胺化反应
imatinib
synthesis
process improvement
amination reaction
