合成N-甲基4-哌啶醇的新工艺

The new synthesis process of N-methyl-4-piperidol

以甲胺溶液和丙烯酸乙酯为原料,经过加成、环合、成盐脱羧高效快捷地合成N-甲基-4-哌啶酮盐酸盐粗品,粗品在Am- berlyst-15(H^+)体系中,经NaBH_4还原得N-甲基-4-哌啶醇,总收率62%。对关键中间产物N,N-双(β-丙烯酸乙酯)甲胺的合成,本文研究了其主要的反应影响因素,如反应温度、通甲胺时间、原料配比,采用最小方差法关联。结果表明,最佳反应条件为:温度70℃,通甲胺时间3 h,原料配比3:1。

N-methyl-4-piperidol was synthesized efficiently and fast with methylamine and ethyl acrylate as raw materials via a series of addition, Dieckmann condensation,hydrolysis decarboxylafion and reduction reactions. The total yield of this procedure was 62%. As to the major intermediate product N, N-double（β-ethyl acrylate）methylamine, the key factors affecting the reaction such as reacting temperature, period of aerating methylamine, ratio of raw materials were studied in this paper, and the results were correlated using minimum covariance method. The experimental and calculated results both showed that the best reacting condition was the reacting temperature 70℃ , period of aerating methylamine 3 h, ratio of raw materials 3： 1.