1-(2,3-二氯苯基)哌嗪的合成及其工艺研究

Research on the preparation method of 1-(2,3-(dichloro-)phenyl)piperazine

1-(2,3-二氯苯基)哌嗪是一种重要的医药中间体,本文采用了两条合成路线,一是以2,6-二氯硝基苯和无水哌嗪为原料,经过烃化、乙酰化、硝基还原、桑德迈尔反应及水解等过程,将硝基转变为氯原子合成该中间体;二是直接用无水哌嗪与2,3-二氯溴苯通过乌尔曼反应合成。第一条路线的总收率以及产品质量都优于第二条路线,其总收率为53.3%。讨论了各步反应的影响因素,最终产物的结构通过红外光谱、核磁共振光谱得到了表征。

1-（2,3-dichlorophenyl）piperazine is a kind of pharmaceutical intermediate. The paper described two synthetic ways. One was to react 2,6-dichloro-nitrobenzene with anhydrous piperazine and then change the nitryl group to chlorine by acidulation, reduction, Sandmeyer and hydrolysis. Another way was to combine directly anhydrous piperazine with 2, 3-dicldoro-bromobenzene through Ullmann reaction. The former was better in terms of the quality and quantity of the final product. The total yield was 53.3%. The factors which influence every single reaction were discussed. The structure of 1- （2,3-dichlorophenyl） piperazine was confirmed by IR and ^1HNMR.