第 46 卷第 6 期 Vol. 46 No. 6 2016 年 12 月 Dec 2016

所属栏目：医药及中间体 微波催化重排法制备对氨基苯乙酮

阎 峰，胡 壮*，王 政，张寒冰，毕 寒，卓桢成，关 瑾 （沈阳化工大学 应用化学学院，辽宁 沈阳 110142）

摘　要：以乙酰苯胺为原料，中性氧化铝为载体，在无水氯化铝的催化下，于微波反应器内发生Fries重排反应。粗产品经盐酸水解、水蒸气蒸馏的方式除去未反应物，并通过兴斯堡反应鉴定反应结果。经红外光谱和核磁共振氢谱对产物结构进行了表征，再结合测定熔点、颜色等物理性质证明了产物为对氨基苯乙酮。通过改变载体用量、催化剂用量和反应时间等条件，探究发现在800 w微波照射下反应时间为12 min，当m（乙酰苯胺）∶m（氯化铝）∶m（氧化铝）=1∶2∶20时，收率68%。

关键词：对氨基苯乙酮；微波催化法；重排反应；兴斯堡反应

中图分类号：O622.4　　文献标识码：A　　文章编号：1009-9212（2016）06-0046-04

Synthesis of P-Aminoacetophenone by Microwave Catalytic Rearrangement

YAN Feng, HU Zhuang*, WANG Zheng, ZHANG Han-bing, ZHUO Zhen-cheng, GUAN Jin (Applied chemistry college, Shengyang university of chemical technology, Shengyang 110142, China)

Abstract：The Fries rearrangement reaction was carried out in the microwave reactor with acetaldehyde as the raw material and neutral aluminum oxide as the carrier under the catalysis of anhydrous aluminum chloride. The resulting product was hydrolyzed by hydrochloric acid, and the unreacted material was removed by steam distillation. The reaction results were identified by Hinsburg reaction. The structure of the product was characterized by IR and 1H NMR. The product was identified as p-aminoacetophenone according to the melting point, color and other physical properties. The effects of the amount of catalyst, the amount of catalyst and the reaction time on the yield were investigated. It was found that the reaction time was 12 min under 800w microwave irradiation, and the highest yield was 68% when acetanilide: aluminum chloride: alumina ratio was 1:2:20(mass ratio).

Key words：P-aminoacetophenone; microwave catalysis; rearrangement reaction; hinsberg reaction

基金项目：辽宁省精细化工协同创新中心协同创新团队资助项目（000053）。

作者简介：阎 峰（1965-），男，辽宁沈阳人，教授，博士，研究方向：精细有机合成。

联 系 人：胡 壮，硕士研究生，研究方向：精细有机合成（E-mail：3446538391@qq.com）。

收稿日期：2016-12-10