长春西汀中杂质A和杂质B的合成

Synthesis of impurities A and B in vinpocetine

目的合成长春西汀中的2个有关物质。方法长春胺在乙醇氢氧化钾溶液中发生水解反应,再经过酸化制得中间体长春胺酸,该中间体在丙酮-碘乙烷溶液中反应制得杂质长春胺乙酯(A);长春胺在甲醇浓硫酸溶液中通过消除反应脱水制得杂质阿扑长春胺(B)。结果与结论合成的有关物质A、B的结构经MS、~1H-NMR、^(13)C-NMR、IR谱确证,HPLC法检测其纯度分别为99.1%、98.9%。杂质A、B可作为长春西汀质量控制的杂质对照品。

For the purpose of quality control of vinpocetine, two related substances were synthesized and characterized. Impurity A was prepared by iodoethane in acetone and vincaminic acid, which was obtained by hydrolysis of vincamine in ethanol potassium hydroxide solution. Impurity B was prepared by dehydration of vincamine in methanol concentrated sulfuric acid solution. The structures of two impurities were characterized by MS, ^1H-NMR, ^13 C-NMR and IR spectra, and the purities （ impurity A 99.1%, impurity B 98.9 % ） were determined by HPLC analysis. Impurities A and B can be used as the reference substances of the related substances in the quality control of vinpocetine.