摘要
由对羟基苯乙酮和2-溴-2-甲基丙酰胺经Williamson醚化反应、Smiles重排反应和水解反应合成了对氨基苯乙酮。通过考察反应溶剂、重排反应温度和物料比对反应收率的影响,确定了优化工艺条件为:N,N-二甲基乙酰胺为溶剂、重排反应温度控制在45-50℃、n(对羟基苯乙酮)∶n(2-溴-2-甲基丙酰胺)=1∶3。最终产品收率达52.1%。目标化合物的结构经1H NMR和IR确证。
4-Aminoacetophenone was synthesized from 4-hydroxyacetophenone and 2-bromo-2-methylpropanamide via Williamson etherification,Smiles rearrangement and hydrolysis reactions.Best result with 52.1% yield was obtained under conditions of reaction dissolvent of DMA,reaction temperature of 45℃~50℃ in rearrangement reaction,molar ratio of 4-hydroxyacetophenone to 2-bromo-2-methylpropanamide of 1 to 3.The structure of the title compound was confirmed by 1H NMR and IR.
出处
《精细化工中间体》
CAS
2013年第1期30-32,58,共4页
Fine Chemical Intermediates