摘要
为控制palbociclib药品质量,从palbociclib原料药中分离并鉴定了3个有关物质:8-环戊基-5-甲基-2-(5-哌嗪-1-基-吡啶-2-基氨基)-8H-吡啶并[2,3-d]嘧啶-7-酮(A)、8-环戊基-5-甲基-6-乙烯基-2-(5-哌嗪-1-基-吡啶-2-基氨基)-8H-吡啶并[2,3-d]嘧啶-7-酮(B)和4-[6-(6-乙酰基-8-环戊基-5-甲基-7-氧代-7,8-二氢吡啶并[2,3-d]嘧啶-2-基氨基)-吡啶-3-基]-哌嗪-1-羧酸叔丁酯(C)。分析了这些有关物质产生的原因并进行了设计合成,其结构经质谱、核磁共振氢谱确证。
To strengthen the quality control of palbociclib, three related substances were separated from the bulk drug. These substances were identified as 8-cyclopentyl-5-methyl-2-( (5-(piperazin-1-yl) pyridin-2-yl) amino) pyrido [2, 3-d] pyrimidin-7(8H) -one(A), 8-cyclopentyl-5-methyl-2-( (5-(piperazin-1-yl) pyridine-2-yl) amino) - 6-vinylpyrido [ 2, 3-d] pyrimidin-7 (8H) -one (B), tert-butyl4-( 6-( ( 6-acetyl-8-cyclopentyl-5-methyl-7-oxo-7, 8- dihydropyrido [2, 3-d] pyrimidin-2-yl) amino) pyridin-3-yl) piperazi-ne-1-carboxylate (C).Based on the structures of the impurities, the possible routes to them were discussed, and their structures were elucidated by were l H NMR and MS.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2015年第6期696-699,共4页
Journal of China Pharmaceutical University