微波辐射固载杂多酸催化合成1-苯基-2-吡咯烷酮

Synthesis of N-phenyl-2-pyrrolidinone under the catalysis of supported heteropolyacid by microwave irradiation

采用微波辐射技术,将硅藻土作载体浸渍于磷钨酸制备成固载杂多酸催化剂,以γ-丁内酯和苯胺为原料合成了1-苯基-2-吡咯烷酮(NPP)。研究了微波工艺条件对反应产率的影响,并用元素分析、红外光谱、核磁共振等手段对产物进行了结构分析。实验结果表明,硅藻土固载磷钨酸催化剂在NPP的合成中显示良好的催化效果,微波辐射制备产物的结构并没有明显的差异,实验筛选的最佳工艺条件为:磷钨酸负载量17.6%、催化剂质量分数1.5%、微波功率325 W、辐射时间14 min、γ-丁内酯与苯胺摩尔比1.0∶1.25。在此条件下NPP产率达96%以上,反应速率提高近10倍。

A supported heteropolyacid catalyst, prepared by soaking diatomite on tungstophosphoric acid, was used to synthesize N-phenyl-2-pyrrolidinone （NPP） by microwave irradiation from gamma hutyrolactone and aniline. The effects of microwave processing conditions on the yield of NPP were studied and the structure was analyzed by IR, ^1 HNMR and elementary analysis. The results indicated that the catalyst performed very well in synthesizing NPP and the change of its structure was insignificant after irradiation. The optimum conditions are as follows： load quantity of tungstophosphoric acid： 17.6%, quantity of catalyst （mass fraction） ：1. 5 %, microwave power： 325W, irradiation time： 14min, molar ratio of gamma butyrolaetone to aniline： 1.0：1. 25. Yield of NPP reached over 96% with about 10-fold rise of reaction speed.