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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12min,当m(乙酰苯胺)∶m(氯化铝)∶m(氧化铝)=1∶2∶20时,收率68%。
With acetanilide as raw material and neutral alumina as carrier, Fries rearrangement reaction occurred in the microwave reactor under the catalysis of anhydrous aluminum chloride. The crude product was hydrolyzed by hydrochloric acid, steam distilled to remove the unreacted material, and the result of the reaction was identified by the method of Fortsburg reaction. The structure of the product was characterized by IR and 1H-NMR and the product was identified as p-aminoacetophenone by physical properties such as melting point and color. By changing the amount of carrier, the amount of catalyst and the reaction time and other conditions, it was found that the reaction time is 12min when the microwave irradiation time is 800min, when m (acetanilide): m (aluminum chloride): m 20, the yield was 68%.