| 液相色谱/质谱联机研究还原烷基化合成3-(β-羟乙基砜基)N-乙基苯胺的反应历程 |
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| 引用本文： | 张蓉,吴祖望,林乐森,杨海燕.液相色谱/质谱联机研究还原烷基化合成3-(β-羟乙基砜基)N-乙基苯胺的反应历程[J].色谱,2000,18(6):532-535. |
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| 作者姓名： | 张蓉 吴祖望 林乐森 杨海燕 |
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| 作者单位： | 大连理工大学染料表面活性剂精细化工合成国家重点实验室!辽宁大连116012 |
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| 摘 要： | 3 (β 羟乙基砜基 )苯胺在催化剂镍的存在下与醛发生加氢反应 ,可直接制得 3 (β 羟乙基砜基 )N 乙基苯胺。运用高效液相色谱 /质谱联机系统对反应生成的中间产物进行分析 ,研究了加氢还原烷基化反应的历程。
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| 关 键 词： | 液相色谱/质谱联机 还原烷基化反应 反应历程 3(β羟乙基砜基)苯胺 3(β羟乙基砜基)N乙基苯胺 |
A study on the mechanism of reductive alkylation for preparing 3-(beta-hydroxy-ethyl-sulfonyl) N-ethyl aniline with HPLC/MS] |
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| R Zhang,Z W Wu,L S Lin,H Y Yang.A study on the mechanism of reductive alkylation for preparing 3-(beta-hydroxy-ethyl-sulfonyl) N-ethyl aniline with HPLC/MS][J].Chinese Journal of Chromatography,2000,18(6):532-535. |
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| Authors: | R Zhang Z W Wu L S Lin H Y Yang |
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| Institution: | State Key Laboratory of Dye and Surfactant Fine Chemicals, Dalian University of Technology, Dalian 116012, China. |
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| Abstract: | Hydrogenating 3-(beta-hydroxy-ethyl-sulfonyl)-aniline and acetaldehyde in the presence of Raney Nickel as a catalyst, 3-(beta-hydroxy-ethyl-sulfonyl)-N-ethyl-aniline was obtained with 98% conversion and 95% monoalkylation selectivity under optimum conditions. By using high performance liquid chromatography/mass selective detection technique to characterize the structures of the products, the mechanism of reductive alkylation is proposed. From the intermediates determined, it is shown that the reaction mechanism would go via an unstable N-alpha-hydroxyethylaniline derivative and Schiff base stage. After hydrogenation of Schiff base, finally the product 3-(beta-hydroxyethyl-sulfonyl)-N-ethyl aniline was formed. |
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| Keywords: | NULL |
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