有机化学 ›› 2009, Vol. 29 ›› Issue (05): 802-805. 上一篇    下一篇

研究简报

1,2-二甲基咪唑啉的合成及表征

徐文清a ; 聂万丽*,a; Borzov Maxim V.a,b; 马兵锋a   

  1. (a西北大学化学系 西安 710069)
    (b国立莫斯科大学化学系 莫斯科 119992)
  • 收稿日期:2008-07-02 修回日期:2008-10-23 发布日期:2009-05-20
  • 通讯作者: 聂万丽

Synthesis and Charaterization of 1,2-Dimethylimidazoline

Xu, Wenqinga ; Nie, Wanli*,a ; Borzov Maxim V.a,b; Ma, Bingfenga
  

  1. (a Department of Chemistry, Northwest University, Xi’an 710069)
    (b Department of Chemistry, Moscow State University, Moscow 119992)
  • Received:2008-07-02 Revised:2008-10-23 Published:2009-05-20
  • Contact: Nie, Wanli

对1,2-二甲基咪唑啉的合成进行了详细研究. 以甲胺水溶液和2-溴乙胺氢溴酸盐(1)为原料进行反应, 在两种原料物质的量之比为5∶1, 缓缓回流12 h的条件下, 得到N-甲基乙二胺(2), N-甲基乙二胺经过乙酸化得到N-甲基-N,N′-二乙酰基乙二胺(3), 然后, N-甲基-N,N′-二乙酰基乙二胺和氧化钙在高温下关环得到1,2-二甲基咪唑啉(4). 并对所得到的产物1,2-二甲基咪唑啉经元素分析, 1H NMR, IR和GC-MS得到了表征.

关键词: 水解, N-甲基-N,N′-二乙酰基乙二胺, 成环反应, 1,2-二甲基咪唑啉

Here a convenient and comparatively cheap route to DMI was provided, which includes that (a) N-methyl ethylenediamine (2) was prepared from aqueous methylamine solution and 1-amino-2-bromo- ethane hydrobromide (1) (molar ratio 5∶1) under gentle reflux during 12 h, (b) N-methyl- N,N′-diace- tylethylenediamine (3) was obtained via direct acetulation of 2 with acetic acid, and (c) the target molecule 1,2-dimethylimidazoline (4) was prepared by CaO catalyzed cyclization of 3 at elevated temperature. All compounds were characterized by elemental analysis, 1H NMR, IR and GC-MS techniques.

Key words: cyclization, 1,2-dimethylimidazoline, hydrolysis, N-methyl-N,N′-diacetylethylenediamine