4-氨基-N-甲基哌啶-1-甲酰胺盐酸盐的合成

Synthesis of 4-Amino-N-methylpiperidine-1-carboxamide Hydrochloride

以哌啶-4-基氨基甲酸叔丁酯和甲氨基甲酰氯为原料,通过N-酰基化和脱Boc保护两步反应合成目标化合物4-氨基-N-甲基哌啶-1-甲酰胺盐酸盐,通过1HNMR、ESI-MS对其结构进行表征,并对脱Boc保护反应条件进行了优化。确定最优脱Boc保护反应条件为:氯化氢/乙酸乙酯用量n(氯化氢/乙酸乙酯)∶n(1-(甲氨基甲酰)哌啶-4-基氨基甲酸叔丁酯)为2.0∶1、反应温度25℃、反应时间1.0 h,在此条件下,目标化合物收率达到86.5%。

Using tert-butyl piperidin-4-ylcarbamate and methylcarbamic chloride as raw materials,we synthesized target compound 4-amino-N-methylpiperidine-1-carboxamide hydrochloride by a two-step reaction,involving N-acylation reaction and Boc-group deprotection reaction.Moreover,we characterized the structure of the target compound by 1HNMR and ESI-MS,and optimized the Boc-group deprotection reaction conditions.The results show that the optimal Boc-group deprotection reaction conditions are determined as follows:the n(hydrogen chloride/ethyl acetate)∶n(tert-butyl piperidin-1-methylcarbamyl-4-ylcarbamate)of 2.0∶1,the reaction temperature of 25℃,and the reaction time of 1.0 h.Under above conditions,the yield of the target compound reaches 86.5%.