摘要
以甲胺溶液和丙烯酸乙酯为原料,经过加成、环合、成盐脱羧合成N-甲基-4-哌啶酮。对合成工艺进行了优化和改进,确定了较佳加成反应温度为50℃,加成溶剂为三乙胺,缩合反应双酯与钠的较佳摩尔配比为1:1.4。产品总收率由文献值的53%提高到59.7%(以丙烯酸乙酯计算)。目标化合物经核磁共振分析确认。
N-methyl-4-piperidone was synthesized with methylamine and ethyl acrylate as raw materials via a series of addition, dieckmann condensation and hydrolysis decarboxylafion reactions The synthetic process and after-treatment were optimized and improved. The total yield of this procedure was increased from 53% to 59.7%. And the product was identified by IHNMR .