论文部分内容阅读
目的为了完善与强化对原料药雷贝拉唑钠的质量控制,合成雷贝拉唑钠有关物质。方法以2-巯基-1H-苯并咪唑和2-氯甲基-4-(3-甲氧基丙氧基)-3-甲基吡啶盐酸盐为原料,合成2-[[[4-(3-甲氧基丙氧基)-3-甲基吡啶-2-基]甲基]硫代]-1H-苯并咪唑(1)和2-[[[4-(3-甲氧基丙氧基)-3-甲基-1-氧代吡啶-2-基]甲基]磺酰基]-1H-苯并咪唑(3);以雷贝拉唑为原料,合成2-[[[4-(3-甲氧基丙氧基)-3-甲基-2-吡啶基]甲基]磺酰基]-1H-苯并咪唑(2)。结果与结论目标化合物的结构经核磁、质谱确证,纯度均大于99.8%,可作为质量控制的标准品。本实验反应条件温和、生成副产物较少、操作简单,并且采用双氧水为氧化剂,降低了成本、减少了环境污染。
Purpose In order to improve and strengthen the quality control of raw material drug rabeprazole sodium, synthetic sodium rabeprazole related substances. Methods 2 - [[[4- (3-methoxypropoxy) -3-methylpyridine hydrochloride was synthesized from 2-mercapto-1H-benzimidazole and 2-chloromethyl- (3-methoxypropoxy) -3-methylpyridin-2- yl] methyl] thio] -1H-benzimidazole (1) and 2- [[[4- Propoxy) -3-methyl-1-oxopyridin-2-yl] methyl] sulfonyl] -1H-benzimidazole (3) 4- (3-methoxypropoxy) -3-methyl-2-pyridyl] methyl] sulfonyl] -1H-benzimidazole (2). Results and Conclusion The structures of the target compounds were confirmed by NMR and mass spectrometry. The purity of the target compounds was more than 99.8%, which could be used as a standard for quality control. The reaction conditions of the experiment are mild, less by-products are formed, the operation is simple, and the hydrogen peroxide is used as the oxidant, which reduces the cost and reduces the environmental pollution.