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以4-甲基苯甲酸为起始原料,经α-位溴化、胺化后不经分离直接酸化制得4-(4-甲基哌嗪-1-甲基)苯甲酸二盐酸盐.考察了溴化剂、引发剂对溴化反应及原料配比、反应温度、反应时间等对胺化过程的影响.得到的工艺条件为:①N-溴代丁二酰亚胺(NBS)为溴化剂、过氧化苯甲酰(BPO)为引发剂,4-溴甲基苯甲酸收率为88.7%;②n(4-溴甲基苯甲酸)∶n(N-甲基哌嗪)=11∶.2,碳酸氢钠为缚酸剂,反应温度20～25℃,反应时间8 h,产品收率81.5%.通过熔点、红外光谱、核磁共振氢谱确定了目标化合物的结构.
Starting from 4-methylbenzoic acid, 4- (4-methylpiperazin-1-ylmethyl) benzoic acid dihydrochloride was obtained by α-position bromination and amination without direct acidification The effects of bromination agent, initiator on the reaction of bromination and the ratio of raw materials, reaction temperature and reaction time on the amination process were investigated.The process conditions were as follows: ① N-bromosuccinimide (NBS) was Bromination agent, benzoyl peroxide (BPO) as initiator, the yield of 4-bromomethylbenzoic acid was 88.7%; ②n (4-bromomethylbenzoic acid) The structure of the target compound was confirmed by melting point, FTIR and 1HNMR. The reaction temperature was 20 ~ 25 ℃, the reaction time was 8 h and the product yield was 81.5%.