摘 要: 目的 研究丁酸氯維地平主要雜質(zhì)的結(jié)構(gòu)和產(chǎn)生的原因。方法 以3-羥基丙腈為起始原料，經(jīng)過酯化、縮合、水解、取代反應(yīng)制備目標(biāo)化合物。用液-質(zhì)聯(lián)用法推導(dǎo)該雜質(zhì)結(jié)構(gòu)。結(jié)果 按照設(shè)計路線，合成出丁酸氯維地平主要雜質(zhì)。結(jié)論 經(jīng)1H-NMR確證目標(biāo)化合物結(jié)構(gòu)為4-(2,3-二氯苯基)-1-4-二氫-2-6-二甲基-3,5-吡啶二羧酸雙(1-氧代丁氧基)甲酯。

Abstract: Objective To identify the structure and cause for product of the main impurity of cleviprex butyrate. Methods LC-MS was used to speculate the main impurity. The target compound was synthesized via esterification, condensation, hydrolization substitution, using 3-hydroxypropionitrile as starting material. Rusults The main impurity of cleviprex butyrate was synthesized by the design route. Conclusion 1H-NMR is used to confirm the target compound, the structure is bis (butyryloxymethyl) 4-(2,3-dichloro-phenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate.