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有机化学
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有机化学 ›› 2006, Vol. 26 ›› Issue (01): 134-138. 上一篇    

研究简报

N-乙氧羰基-N'-3-吡啶基硫脲的合成及其超分子晶体结构

张有明1，杨莉梓1，林奇1，魏太保*,1，王大奇2   

  1. (1西北师范大学化学化工学院 甘肃省高分子材料重点实验室 兰州 730070)
    (2聊城大学化学系 聊城 252059)
  • 收稿日期:2005-04-06 修回日期:2005-07-18 发布日期:2005-12-31
  • 通讯作者: 魏太保

Synthesis and the Crystal Structure of N-Ethoxycarbonyl- N'-(3-pyridyl)thiourea

ZHANG You-Ming1,YANG Li-Zi1,LIN Qi1,WEI Tai-Bao*,1,WANG Da-Qi2   

  1. (1 Gansu Key Laboratory of Polymer Materials, College of Chemistry and Chemical Engineering,
    Northwest Normal University, Lanzhou 730070)
    (2 Department of Chemis-try, Liaocheng University, Liaocheng 252059)
  • Received:2005-04-06 Revised:2005-07-18 Published:2005-12-31
  • Contact: WEI Tai-Bao

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以N,N,N',N'-四甲基乙二胺(TMEDA)为催化剂, 通过氯甲酸乙酯与硫氰酸钾反应合成了中间体乙氧羰基异硫氰酸酯, 后者不需分离直接与3-氨基吡啶反应, 得到N-乙氧羰基-N'-3-吡啶基硫脲. 该产物用EA, IR, 1H NMR进行了表征, 经X射线单晶衍射法确定了其单晶结构, 晶体结构表明, 晶体属于单斜晶系, P2(1)/c空间群, 晶胞参数: a＝1.0333(6) nm, b＝0.7118(4) nm, c＝1.5160(8) nm, α＝γ＝90.00°, β＝98.517(8)°, V＝1.1028(10) nm3, Z＝4. 晶体中硫脲分子通过分子间氢键的相互作用形成了一维链状超分子结构, 由于范德华力作用形成沿b轴延伸的层状结构.

关键词: 3-氨基吡啶, 晶体结构, 合成

Ethyl chloroformate was treated with potassium thiocyanate in ethyl acetate in the presence of a catalysis N,N,N',N'-tetramethylethylenediamine to produce the ethoxycarbonylisothiocyanate. This compound can directly react with 3-amino-pyridine without isolation to afford N-ethoxycarbonyl-N'-(3-pyridyl)- thiourea. The compound crystallized in the monoclinic system with space group P2(1)/c and a＝1.0333(6) nm, b＝0.7118(4) nm, c＝1.5160(8) nm, α＝γ＝90.00°, β＝98.517(8)°, V＝1.1028(10) nm3, Z＝4. The thiourea molecule formed a supermolecule by hydrogen banding.

Key words: crystal structure, synthesis, 3-aminopyridine