7,8-二甲氧基-3-(3-碘丙基)-1,3-二氢-2H-3-苯并氮杂-2-酮的制备

Preparation of 7,8-dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one

目的合成抗心绞痛的新药伊伐布雷定的关键中间体7,8-二甲氧基-3-(3-碘丙基)-1,3-二氢-2H-3-苯并氮杂--2-酮。方法以3,4-二甲氧基苯乙酸为原料,经卤化、酰化、环合、烷基化、碘取代等反应制得目标化合物。结果五步反应总收率为63.6%,产物经MS1、HNMR确证结构。结论所用工艺路线具有原料易得、操作简便、收率较高的特点,适用于该中间体的放大制备。

OBJECTIVE To synthesize 7,8-dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one,a key intermediate of Ivabradine(a new antianginal drug).METHODS The target compound was synthesized from 3,4-dimethoxyphenylacetic acid via halogenation,acylation,cyclization,alkylation and iodine substitution reaction.RESULTS Chemical structure of compounds was confirmed by MS and 1HNMR and overall yield was 63.6%.CONCLUCION The materials are available and the procedures are manipulated easily which make the route pra...