有机化学 ›› 2007, Vol. 27 ›› Issue (02): 285-288. 上一篇    

研究简报

4,5-二[2-(邻甲酰苯氧基)乙硫基]-1,3-二硫环戊烯-2-酮的合成及晶体结构

赵邦屯*,a,陈俊清b,渠桂荣*,b   

  1. (a洛阳师范学院化学系 洛阳 471022)
    (b河南师范大学化学与环境科学学院 新乡 453002)
  • 收稿日期:2006-02-20 修回日期:2006-10-24 发布日期:2007-01-30
  • 通讯作者: 渠桂荣

Synthesis and Structure of 4,5-Bis[2-(ο-formylphenoxy)ethylthio]-1,3-dithiol-2-one

ZHAO Bang-Tun*,a, CHEN Jun-Qingb, QU Gui-Rong*,b   

  1. (a Department of Chemistry, Luoyang Normal University, Luoyang 471022)
    (b College of Chemistry and Environmental Science, Henan Normal Univer-sity, Xinxiang 453002)
  • Received:2006-02-20 Revised:2006-10-24 Published:2007-01-30
  • Contact: QU Gui-Rong

以水杨醛与1,2-二溴乙烷为反应物, 乙腈为溶剂, 在无水K2CO3存在下合成了2-溴乙氧基水杨醛(1), 1和二-(1,3-二硫杂环戊烯-2-硫酮-4,5-二硫)合锌酸四乙基铵盐在乙腈中回流, 得到新型的四硫富瓦烯(TTF)前体(2). 在Hg(OAc)2存在下, 2可转化为4,5-二[2-(邻甲酰苯氧基)乙硫基]-1,3-二硫环戊烯-2-酮(3), 其结构经1H NMR, FT-IR, 元素分析和单晶X射线衍射分析得到确证.

关键词: 4,5-二[2-(邻甲酰苯氧基)乙硫基]-1,3-二硫环戊烯-2-酮, 四硫富瓦烯(TTF)前体, 晶体结构

2-Bromoethoxybenzaldehyde (1) was prepared by the reaction of salicyladehyde with 1,2-dibromoethane in the presence of anhydrous K2CO3. 1 reacted with di(tetraethylammonium) bis(1,3- dithiol-2-thione-4,5-dithiolate)zincate in refluxing with CH3CN to give a new precursor (2) of Tetrathiafulvalene (TTF). In the presence of Hg(OAc)2, 2 was con-versed to 4,5-bis[2-(o-formylphenoxy)ethylthio]-1,3- dithiol-2-one (3), which was identified and characterized by 1H NMR, IR and ele-mental analysis along with X-ray diffraction analysis.

Key words: crystal structure, tetrathiafulvalene (TTF) precursor, 4,5-bis[2-(o-formylphenoxy)ethylthio]-1,3-dithiol-2-one