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有机化学
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有机化学 ›› 2007, Vol. 27 ›› Issue (11): 1409-1413. 上一篇    下一篇

研究简报

刺乌头碱氢溴酸盐的合成及晶体结构

张继a，孙文秀a，温慧慧a，刘汉士a
李红坤a，郁开北b，王云普*,a   

  1. (a西北师范大学高分子研究所 兰州 730070)
    (b中国科学院成都分院分析中心 成都 610041)
  • 收稿日期:2006-08-10 修回日期:2007-03-13 发布日期:2007-10-20
  • 通讯作者: 王云普

Synthesis and Crystal Structure of Lappaconitine Hydrobromide

ZHANG Jia,SUN Wen-Xiua,WEN Hui-Huia,LIU Han-Shia
LI Hong-Kuna,YU Kai-Beib,WANG Yun-Pu*,a   

  1. (a Institute of Polymers, Northwest Normal University, Lanzhou 730070)
    (b Analysis and Testing Center Chengdu Branch, Chinese Academy of Sci-ences, Chengdu 610041)
  • Received:2006-08-10 Revised:2007-03-13 Published:2007-10-20
  • Contact: WANG Yun-Pu

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被引次数

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报道了以双溴代烷烃和刺乌头碱合成刺乌头碱氢溴酸盐的方法. 用元素分析、红外光谱、高分辨质谱和核磁共振进行了表征. 并用X射线单晶衍射确定了标题化合物的绝对构型. 晶体结构表明, 该化合物通过分子间氢键形成了网状类似超分子结构. 晶体属于单斜晶系, P21空间群, 晶胞参数: a＝1.0619(2) nm, b＝1.2196(3) nm, c＝1.2282(2) nm, β＝90.87(1)°, V＝1.59037(54) nm3, Z＝2, Dm＝1.428 g/cm－3, F(000)＝720.0, µ＝1.349 mm－1. 环 A, B, C, D, E和F分别呈船式、椅式、信封式、船式、船式和信封式. 其绝对构型被确定为1S,4S,5S,7S,8S,9S,10S,11S,13R,14S,16S,17R.

关键词: 刺乌头碱氢溴酸盐, 绝对构型, 晶体结构, 表征, 合成

A method for the synthesis of lappaconitine hydrobromide by the reaction of dibromoalkyl with lappaconitine is presented. Lappaconitine hydrobromide was determined by IR, 13C NMR, HRMS spectra, elemental analysis and X-ray diffraction analysis. Through intermolecular hydrogen bonding, the similar super molecule netlike structure is formed. Crystal data: monoclinic, P21, a＝1.0619(2) nm, b＝1.2196(3) nm, c＝1.2282(2) nm, β＝90.87(1)°, V＝1.59037(54) nm3, Z＝2, Dm＝1.428 g/cm－3, F(000)＝720.0, μ＝1.349 mm－1. Rings A, B, C, D, E and F present boat, chair, envelope, boat, boat and envelope forms, respectively. The stereo absolute configuration of lappaconitine hydrobromide was determined as 1S,4S,5S,7S,8S, 9S,10S,11S,13R,14S,16S,17R.

Key words: absolute configuration, crystal structure, characterization, synthesis, lappaconitine hydrobromide