一锅法合成雷贝拉唑钠  

Preparation of rabeprazole sodium by a single-pot method

作　　者：华坤鹏 谭淑珍[1] 王成[1] 王述维 

机构地区：[1]长沙理工大学化学与生物工程学院,湖南长沙410114 [2]湖南如虹制药有限公司,湖南岳阳414300

出　　处：《化学工程师》2016年第3期8-11,共4页Chemical Engineer

基　　金：湖南省教育厅资助科研项目(14A012)

摘　　要：开发了一锅法合成雷贝拉唑钠的新工艺,以2-氯甲基-4-(3-甲氧基丙氧基)-3-甲基吡啶盐酸盐(SM1)和2-巯基苯并咪唑(SM2)为起始原料,以二氯甲烷和Na OH水溶液为反应介质,经缩合反应所得溶液不进行分离,直接用NaClO进行氧化得到雷贝拉唑钠粗品,再经重结晶得到高纯度的雷贝拉唑钠。通过试验对缩合反应溶剂和投料比,对氧化反应的温度、氧化剂用量等因素进行了优化,得到了较佳的制备条件,在此条件下雷贝拉唑钠纯度大于99.5%、总收率达到83%以上,产品结构经红外光谱(FTIR)、核磁共振谱(NMR)进行了确证。A novel method for preparation of rabeprazole sodium was developed by using a single-pot process,in which 2-chloromethyl-4-（3-methoxypropoxy）-3-methylpyridine hydrochloride（SM1） and 2-mercaptobenzimidazole（SM2） were used as raw materials, a mixed solution of sodium hydroxide in water and dichloromethane was used as reaction medium, the mixture obtained from condensation reaction of SM1 and SM2 was oxidized di-rectly by sodium hypochlorite to form the crude product of rabeprazole sodium, followed by recrystallization to pro-duce high pure rabeprazole sodium. The reaction medium and molar ratio of raw materials for condensation reac-tion, reactive temperature and dosage of oxidant for oxidation reaction were investigated, and the optimized condi-tion was obtained. Under this condition, the target compound was obtained with the purity of more than 99.5% and the yield of more than 83%, and its structure was confirmed by FTIR and NMR.

关 键 词：雷贝拉唑钠 一锅法 合成 

分 类 号：TQ460.63[化学工程—制药化工] TQ227.3