N-苯基吡咯烷的微波合成工艺研究

Study on microwave-assisted synthetic technology of N-phenylpyrrolidine

摘要:

以苯胺和1,4-丁二醇二甲磺酸酯为原料，在缚酸剂存在条件下发生微波反应，生成N-苯基吡咯烷。采用单因素实验及正交实验法考察了溶剂、缚酸剂、温度、时间、原料配比、功率对反应收率的影响，获得最佳的工艺条件：以水做溶剂，碳酸钾做缚酸剂，反应温度100 ℃，时间60 min，原料配比：n(苯胺)∶n(1,4-丁二醇二甲磺酸酯)∶n(碳酸钾) = 1:1.3:1.3，微波功率200 W时，收率可达78.6 %。该工艺条件具有反应迅速、条件温和、处理简单、产品纯度高、环境友好等优点，具有较好的工业化应用前景。

Abstract:

N-Phenylpyrrolidine is synthesized from aniline and 1,4-butanediol dimethanesulfonate by microwave-assisted reaction in the presence of deacid reagent. Through single factor and orthogonal experiments, various factors influencing the yield are investigated. The optimal reaction conditions are obtained as follows: n(aniline) : n(1,4-butanediol dimethanesulfonate): n(potassium carbonate) = 1:1.3:1.3, reaction time 60 minutes, microwave power 200 W, reaction temperature 100 ℃, the yield 78.6 % of N-phenylpyrrolidine can be achieved in water under this condition. The optimal process conditions have advantages of rapid reaction, mild conditions, simple operation, high product purity, and environment-friendliness. So it is suitable for industrialized production.