N-苯基吡咯烷的微波合成

Microwave-assisted Synthetic Technology of N-Phenylpyrrolidine

以苯胺和1,4-丁二醇二甲磺酸酯为原料,在缚酸剂存在下微波反应生成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,获得最佳工艺条件为:以水作溶剂,碳酸钾作缚酸剂,反应温度100℃,辐照时间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,在该条件下收率可达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。

N-Phenylpyrrolidine was synthesized from aniline and 1,4-butanediol dimethanesulfonate by the microwave-assisted reaction in the presence of deacid reagent.Through the single factor and orthogonal experiments,various factors influencing the yield were investigated.The optimal reaction conditions were obtained as follows：n（aniline）∶ n（1,4-butanediol dimethanesulfonate）∶ n（potassium carbonate）=1∶ 1.3∶ 1.3,reaction time 60 min,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 the advantages of rapid reaction,mild conditions,simple operation,high product purity,and environment-friendliness.