| 对氨基苯乙酮新合成方法的研究 |
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| 引用本文： | 孙冰,杜婷婷,吴梦琦,郭丹慧,胡春.对氨基苯乙酮新合成方法的研究[J].精细化工中间体,2013,43(1):30-32,58. |
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| 作者姓名： | 孙冰 杜婷婷 吴梦琦 郭丹慧 胡春 |
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| 作者单位： | 沈阳药科大学制药工程学院,辽宁沈阳,110016 |
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| 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4550℃、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。
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| 关 键 词： | 合成 对羟基苯乙酮 对氨基苯乙酮 Smiles重排 |
Novel Synthesis of 4-Aminoacetophenone |
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| SUN Bing,DU Ting-ting,WU Meng-qi,GUO Dan-hui,HU Chun.Novel Synthesis of 4-Aminoacetophenone[J].Fine Chemical Intermediates,2013,43(1):30-32,58. |
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| Authors: | SUN Bing DU Ting-ting WU Meng-qi GUO Dan-hui HU Chun |
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| Affiliation: | (School of Pharmaceutical Engineering,Shenyang Pharmaceutical University,Shenyang 110016,China) |
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| Abstract: | 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. |
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| Keywords: | synthesis 4-hydroxyacetophenone 4-aminoacetophenone smiles rearrangement |
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