摘要
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.
4-[（4-Methylpiperazin-1-yl）methyl]benzoic acid dihydrochloride was synthesized from 4-methylbenzoic acid via the α-bromination and acidification after amination without separation.The effects of the bromine agent and initiator on the bromination,and that of material ratio,temperature and time on amination were investigated.The optimized conditions were：bromosuccinimide as bromine agent,benzoyl peroxide as the initiator,the yield of 4-（bromomethyl）benzoic acid was close to 88.7%;the ratio of 4-（bromomethyl）benzoic acid to 1-methylpiperazine 1∶1.2,sodium bicarbonate as the acid binding agent,the reaction temperature ranges from 20～25 ℃,the reaction time 8 h.The yield of product under these optimum reaction conditions was up to 81.5%.The structure of the product was confirmed by melting point,IR and 1HNMR.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2010年第11期1100-1102,1120,共4页
Fine Chemicals
