化工进展

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2,6-二氨基-3-硝基甲苯的合成

吴纯鑫,李婷婷,赵德明,张建庭,金宁人   

  1. 浙江工业大学化学工程与材料学院,浙江 杭州 310012
  • 出版日期:2014-08-05 发布日期:2014-08-05

Synthesis of 2,6-diamido-3-nitrotoluene

WU Chunxin,LI Tingting,ZHAO Deming,ZHANG Jianting,JIN Ningren   

  1. College of Chemical Engineering and Materials Science,Zhejiang University of Technology,Hangzhou 310014,Zhejiang,China
  • Online:2014-08-05 Published:2014-08-05

摘要: 以2,6-二氨基甲苯为原料,酰化反应得到2,6-二乙酰氨基甲苯,混酸硝化,水解得到2,6-二氨基-3-硝基甲苯(DANT)目标产品。纯度97.6%、总收率达62%以上。考察了溶剂用量、反应时间,反应温度等因素的影响,优化选择了各反应的较佳工艺参数。酰化反应中,乙酸酐与乙酸的体积比为 1∶2,温度80℃,反应时间2h;硝化反应中,浓硝酸与2,6-二乙酰氨基甲苯的摩尔比1.38∶1,温度为10℃。105℃回流,酸性水解,得产品。产品经13C-NMR、MS 进行了结构表征。

关键词: 2, 6-二氨基-3-硝基甲苯, 2, 6-二氨基甲苯, 合成, 硝化

Abstract: 2,6-diamido-3-nitrotoluene(DANT)was synthesized from 2,6-diamidotoluene,via acylation and nitration. The target compound 2,6-diamido-3-nitrotoluene was got with purity 97.6% and total yield 62%. The effects of solvent amount,reaction time and reaction temperature were investigated,and the optimal process parameters were as follows:the volume ratio of acetic anhydride and acetic acid 1∶2,reaction temperature 80℃,reaction time 2h in acylation reaction;the ratio of concentrated nitric acid and 2,6-acetamidotoluene 1.38∶1,reaction temperature 10℃ in nitration. Then the product was obtained through hydrolysis at 105℃. The product was characterized with 13C-NMR and MS.

Key words: 2,6-diamido-3-nitrotoluene, 2,6-diamidotoluene, synthesis, nitration

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