有机化学 ›› 2012, Vol. 32 ›› Issue (04): 786-789.DOI: 10.6023/cjoc1107201 上一篇    下一篇

研究简报

丙酮肟氧化偶联合成2,3-二甲基-2,3-二硝基丁烷反应的研究

张胜建, 赵迎宪, 张洪   

  1. 浙江大学宁波理工学院 宁波 315100
  • 收稿日期:2011-07-20 修回日期:2011-11-28 发布日期:2012-04-24
  • 通讯作者: 张胜建 E-mail:zsj@nit.zju.edu.cn

Synthesis of 2,3-Dimethyl-2,3-dinitrobutane by Oxidative Coupling of Acetone Oxime

Zhang Shengjian, Zhao Yingxian, Zhang Hong   

  1. Ningbo Institute of Technology, Zhejiang University, Ningbo 315100
  • Received:2011-07-20 Revised:2011-11-28 Published:2012-04-24

以丙酮肟为原料, 在改性TS-1(钛硅分子筛)催化剂催化下, 可用H2O2 氧化偶联合成2,3-二甲基-2,3-二硝基丁烷(DMNB). 在此基础上以丙酮为原料, 在改性TS-1 催化剂催化下, 一锅法进行丙酮氨肟化和氧化偶联反应可制备收率43.2%的DMNB. 该方法简便易操作, 操作安全. 产物结构经1H NMR, 13C NMR 表征.

关键词: 丙酮肟, 氧化偶联, 双氧水, 2,3-二甲基-2,3-二硝基丁烷, 改性TS-1 催化剂

2,3-Dimethyl-2,3-dinitrobutane (DMNB) was prepared by oxidative coupling of acetone oxime with H2O2 over the modified TS-1 catalyst. In one-pot operation, the ammoximation of acetone followed by catalytic oxidative coupling over TS-1 produced the DMNB with yield of 43.2%. The operation is simple and safe. The structures of products were identified by 1H NMR and 13C NMR spectra.

Key words: acetone oxime, oxidative coupling, hydrogen peroxide, 2,3-dimethyl-2,3-dinitrobutane, modified TS-1 catalyst