1-甲基-4-哌啶酮的合成

Synthesis of 1-Methyl-4-piperidone

以甲胺的甲醇溶液和丙烯酸甲酯为原料,经Michael加成、Dieckmann环合和脱羧反应合成得到了1-甲基-4-哌啶酮,并对各步反应的工艺参数进行了优化,在n(丙烯酸甲酯)/n(甲胺)=2.2,n(甲醇钠)/n〔甲基-二-(β-甲氧羰乙基)胺〕=1.14,Michael加成反应温度25℃,Dieckmann环合反应温度80～83℃,脱羧反应温度100～103℃的条件下,1-甲基-4-哌啶酮的总收率为58%,并按该工艺顺利完成了500L反应釜中试。

1-Methyl-4-piperidone was obtained from a methanol solution of methylamine and methyl acrylate through Michael addition, Dieckmann cyclization and decarboxylation. Thus, with n （methyl acrylate）/n （ methylamine ） = 2.2 and n （ sodium methoxide ）/n [ methyl-di- （β-methoxycarbonylethyl） amlne]= 1.14, Michael addition at 25 ℃, Dieckmann cyclization at 80 - 83 ℃ and decarboxylation at 100 - 103 ℃, the total yield of 1-methyl-4-piperidone was 58%. 500 L reactor pilot test was successfully carried out.