2-(甲氨基)-1-苯乙酮盐酸盐的合成研究

Synthesis of 2-methylamino-1-phenyl-ethanone hydrochloride

对2-(甲氨基)-1-苯乙酮盐酸盐的合成工艺进行改进。以2′-溴苯乙酮为起始原料,与两倍当量的N-甲基苄胺进行亲核取代反应得到中间体2-(N-甲基-N-苄基)-氨基-1-苯乙酮(3)。化合物(3)为叔胺化合物,先与α-氯乙基氯甲酸酯(ACE-Cl)反应成酰胺再脱去苄基,即采用α-氯乙基氯甲酸酯法脱去苄基,得到最终化合物2-(甲氨基)-1-苯乙酮盐酸盐(4),两步反应总收率为78%,中间体及终产物的结构均经IR,1H NMR,13 C NMR和HRMS确证。

The synthesis process of the compound of 2-methylamino-1-pheny-ethanone hydrochloride was improved by a simple and efficient operation method.2-(benzyl(methyl)amino)-1-phenylethan-1-one(3)was prepared by a nucleophilic substitution reaction of 2′-bromoacetophenone with two equivalent N-methyl-1-phenylmethanamine.Subsequently,the targeted product 2-methylamino-1-pheny-ethanone hydrochloride(4)was obtained via a substituent debenzylation reaction between ACE-Cl and compound 3.The total yield of 2-methylamino-1-pheny-ethanone hydrochloride in the two-step synthesis method was 78.7%.The structures of intermediates and title product were confirmed by IR,1H NMR,13 C NMR and HRMS.