盐酸利匹韦林顺式异构体Z和杂质X的合成与表征  

Synthesis and Characterization of cis-Isomer Z and Impurity X of Rilpivirine Hydrochloride

作　　者：郭建锋 肖琳霞 屈钦 汪淼 田峦鸢 李莉娥 刘敏 GUO Jianfeng;XIAO Linxia;QU Qin;WANG Miao;TIAN Luanyuan;LI Lie;LIU Min(Yichang Renfu Pharmaceutical Co.,Ltd.,Yichang 443000,China)

机构地区：[1]宜昌人福药业有限责任公司,湖北宜昌443000

出　　处：《化学与生物工程》2023年第2期65-68,共4页Chemistry & Bioengineering

摘　　要：以(E)-3-(4-氨基-3,5-二甲基苯基)丙烯腈为起始物料,通过在氨基氮原子上引入三氟乙酰基等吸电子基团,可以合成较多的盐酸利匹韦林顺式异构体Z(约占50%)和杂质X(约占5%),其结构经1HNMR、13CNMR和MS等确证,并通过HPLC检测其纯度均达到98%以上,杂质X可以作为盐酸利匹韦林杂质对照品,为盐酸利匹韦林的质量研究提供了依据。Taking(E)-3-(4-amino-3,5-dimethylphenyl)acrylonitrile as a starting material, more cis-isomer Z of rilpivirine hydrochloride(about 50%) and impurity X(about 5%) can be obtained by introducing electron-absorbing groups such as trifluoroacetyl group on the amino nitrogen atom.Moreover, the structures of the cis-isomer Z and impurity X are confirmed by ~1HNMR,13CNMR,and MS,and their purity can reach more than 98% by HPLC detection.Impurity X can be used as the impurity reference of rilpivirine hydrochloride.The study provides a basis for the quality study of rilpivirine hydrochloride.

关 键 词：盐酸利匹韦林 合成 吸电子基团 顺式异构体 杂质 

分 类 号：TQ463[化学工程—制药化工]