对硝基甲苯合成3,4-二甲基苯胺的研究

Synthesis of 3,4-Xylidine from 1-Methyl-4-nitrobenzene

以对硝基甲苯为原料,经胺甲基化、水解、还原3步反应合成了目标化合物。通过单因素实验,分析每一步反应的关键影响因素,初步得到适宜的合成条件。最终产物的结构经核磁氢谱、质谱、元素分析进行确证,纯度经气相色谱分析。3,4-二甲基苯胺的总收率56.6%,纯度大于98.5%。该合成路线原料易得,成本较低,操作简单。

3,4-Xylidine is an important pharmaceutical and pesticide intermediate.In the present study,3,4-xylidine is prepared from 1-methyl-4-nitrobenzene by aminomethylation,hydrolysis and hydrogenation reduction reaction.The main factors effecting the above three procedures are investigated through single factor experiments,the optimum condition is obtained.The structure of 3,4-xylidine was confirmed by 1 H-NMR、MS and elementary analysis,and the purity analysis by gas chromatography.The yield and the purity of 3,4-xylidine is 56.6%and 98.5%,respectively.The synthetic method has advantages on readily available materials,low cost,simple operation.