磷酸哌喹杂质7G氯G4G羟基喹啉合成研究  

Research on the synthesis of impurity 7-chloro-4-hydroxyquinoline in piperaquine phosphate

作　　者：李晓花[1] 赵欣[1] 张翠亚 唐静[1] 王艳娇[1,2] LI Xiao-hua;ZHAO Xin;ZHANG Cui-ya;TANG Jing;WANG Yan-jiao(School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xianyang 712046,China;Xianyang Key Laboratory of Molecular Imaging and Drug Synthesis,Xianyang 712046,China)

机构地区：[1]陕西国际商贸学院医药学院,陕西咸阳712046 [2]咸阳市分子影像与药物合成重点实验室,陕西咸阳712046

出　　处：《精细与专用化学品》2024年第10期36-38,共3页Fine and Specialty Chemicals

基　　金：咸阳市分子影像与药物合成重点实验室项目(2021QXNL-PT-0008);陕西省教育厅一般专项科研计划项目(23JK0323)。

摘　　要：报道了磷酸哌喹生产过程中产生的杂质——7-氯-4-羟基喹啉(化合物2)的合成方法。以硅油为脱羧剂,7-氯-4-羟基喹啉-3-羧酸(化合物1)的C-3位发生脱羧反应得到化合物2,其结构经1HNMR和MS表征。考察了影响化合物2收率的主要因素,确定适宜反应条件为:硅油为脱羧剂,在190℃下反应20min。在该条件下,化合物2的收率达到96.8%(以化合物1计)。The synthesis of impurity(compound 2) of piperaquine phosphate was reported.The compound 2 was easily formed through the decarboxylation of the carboxyl group at C-3 position of 7-chloro-4-hydroxyquinoline-3-carboxylic acid(compound 1) by using silicone oil as a deacidification agent.The structures of impurity(compound 2) were confirmed by ~1HNMR and MS.Moreover, the main factors affecting the yield of impurities(compound 2) were investigated, and the appropriate reaction conditions were determined as follows: silicon oil as the decarboxylation agent, reaction at 190℃ for 20min.The yield was up to 96.8%(calculated as compound 1) under this reaction conditions.

关 键 词：磷酸哌喹 杂质 合成 

分 类 号：TQ463[化学工程—制药化工]