中华医学超声杂志

应用化学 ›› 2012, Vol. 29 ›› Issue (01): 80-83.DOI: 10.3724/SP.J.1095.2011.00065

• 研究论文 • 上一篇    下一篇

一种合成3,5-二氨基吡啶及3,5-二甲氧羰基氨基吡啶的新路线

胡炳成*,梁长玉,陆明,戴红升,孙呈郭,徐士超   

  1. (南京理工大学化工学院 南京 210094)
  • 收稿日期:2011-02-21 修回日期:2011-04-08 出版日期:2012-01-10 发布日期:2012-01-10
  • 通讯作者: 胡炳成,教授; Tel/Fax:025-84315030; E-mail:hubingcheng@yahoo.com; 研究方向：有机合成和绿色催化
  • 作者简介:第二作者：梁长玉 南京理工大学    210094
  • 基金资助:
    国家部委基金(HZY09020302-7)资助项目；国家自然科学基金委员会和中国工程物理研究院联合基金资助项目(11076017)

A New Synthetic Route to 3,5-Diaminopyridine and 3,5-Dimethoxycarbonylamino-pyridine

HU Bingcheng*, LIANG Changyu, LU Ming, DAI Hongsheng , SUN Chengguo, XU Shichao   

  1. (School of Chemical Engineering,Nanjing University of Science & Technology,Nanjing 210094)
  • Received:2011-02-21 Revised:2011-04-08 Published:2012-01-10 Online:2012-01-10
  • About author:Changyu Liang    Nanjing University of Science & Technology     

PDF

1750

被引次数

7

摘要：

以3,5-二甲基吡啶为起始原料，经氧化、酰胺化，酰胺在不同的霍夫曼降解条件下合成3,5-二氨基吡啶及3,5-二甲氧羰基氨基吡啶，总收率分别为64%和68%。利用1H NMR、MS/MS、IR等方法对各化合物的结构进行了表征。讨论了氧化反应及霍夫曼降解反应的主要影响因素。反应均在常压下进行，反应条件温和，后处理简单，效率高。

关键词: 二甲基吡啶, 霍夫曼降解, 二氨基吡啶, 二甲氧羰基氨基吡啶, 合成

Abstract:

3,5-Diaminopyridine and 3,5-dimethoxycarbonylamino-pyridine were prepared from 3,5-dimethylpyridine in three steps including oxidation of methyl, amination and Hofmann degradation with the total yield of 64% and 68%, respectively. The reaction conditions of every step were studied and the intermediates and target compounds were characterized by 1H NMR, MS/MS, and IR. The reactions proceed under atmosphere pressure with mild reaction conditions, easy post treatment and high efficiency.

Key words: dimethylpyridine, Hofmann degradation, diaminopyridine, pyridinedicarbonylanmino, synthesis

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