摘要
对现行磷酸氯喹的合成工艺进行研究,以解决原料污染大、收率低、质量差的问题。以4,7-二氯喹啉为起始原料,与2-氨基-5-二乙胺基戊烷直接进行缩合反应,引入一种HPLC中控检测方法监控反应过程;得到的氯喹缩合液,经过一种去杂质方法,再直接与磷酸一锅成盐,制得磷酸氯喹。避免使用高毒性溶剂和催化剂,HPLC中控检测确保反应完全;所得的磷酸氯喹纯度高达99.8%以上;氯喹缩合液与磷酸一锅成盐,收率也得到提升。改进后的工艺绿色环保、操作简单、收率高、产品质量好,更适合工业化生产。
The synthesis process of chloroquine phosphate was studied to solve the problems of high pollution,low yield and poor quality.4,7-dichloroquinoline was used as starting material to directly condense with 2-amino-5-diethylaminopentane,and an HPLC intermediate control method was introduced to monitor the reaction process.Chloroquine phosphate was prepared from chloroquine condensation liquid by a method of removing impurities and then directly salt it with phosphoric acid.Avoid the use of highly toxic solvents and catalysts,HPLC intermediate control test to ensure complete reaction;The purity of chloroquine phosphate was over 99.8%.The condensation solution of chloroquine was combined with phosphoric acid to form salt,and the yield was also improved.The improved process has the advantages of green environmental protection,simple operation,high yield and good product quality,and is more suitable for industrial production.
作者
袁拥军
吴玉祥
滕飞
顾健波
Yuan Yongjun;Wu Yuxiang;Teng Fei;Gu Jianbo(Nantong Jinghua Pharmaceutical Co.,Ltd.,Nantong,Jiangsu 226407,China)
出处
《化工与医药工程》
CAS
2024年第5期22-25,共4页
Chemical and Pharmaceutical Engineering
关键词
医药
磷酸氯喹
工艺研究
medicine
chloroquine phosphate
process research