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.
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)
出处
《化学与生物工程》
CAS
2023年第2期65-68,共4页
Chemistry & Bioengineering
关键词
盐酸利匹韦林
合成
吸电子基团
顺式异构体
杂质
rilpivirine hydrochloride
synthesis
electron-absorbing group
cis-isomer
impurity
