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有机化学
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有机化学 ›› 2005, Vol. 25 ›› Issue (04): 399-404. 上一篇    下一篇

研究论文

四乙酰基二亚硝基六氮杂异伍兹烷水合物(TADNIW•H2O)的合成与晶体结构

吕连营*,1，欧育湘2，王建龙3   

  1. (1石家庄学院化学系 石家庄 050035)
    (2北京理工大学材料科学与工程学院 北京 100081)
    (3华北工学院化学工程系 太原 030051)
  • 收稿日期:2004-03-12 修回日期:2004-10-25 发布日期:2005-03-30
  • 通讯作者: 吕连营

Synthesis and Crystal Strucutre of Tetraacetyldinitroso-hexaazaisowurtzitane (TADNIW•H2O)

LÜ Lian-Ying*,1,OU Yu-Xiang2,WANG Jian-Long3   

  1. (1 Department of Chemistry, Shijiazhuang College, Shijiazhuang 050035)
    (2 School of Materials Science and Engineering, Beijing Institute of Technol-ogy, Beijing 100081)
    (3 Department of Chemical Engineering, North China Institute of Technology, Taiyuan 030051)
  • Received:2004-03-12 Revised:2004-10-25 Published:2005-03-30
  • Contact: LÜ Lian-Ying

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以无机试剂组成的三元复合亚硝解脱苄试剂, 由四乙酰基二苄基六氮杂异伍兹烷(TADBIW)合成了四乙酰基二亚硝基六氮杂异伍兹烷(TADNIW•H2O)——合成高能量密度化合物六硝基六氮杂异伍兹烷(HNIW)和其他高能量密度精细化工产品的另一重要前体. 目标化合物的分子结构用1H NMR, IR, MS及元素分析方法进行结构鉴定. 在乙酸乙酯、丙酮和DMF组成的混合溶剂中制得TADNIW•H2O单晶, 用X射线衍射法测定了目标化合物的晶体结构, 晶体学数据: 单斜晶系, 空间群P21/n; 晶胞参数: a＝1.0738(2) nm, b＝1.4870(3) nm, c＝1.1185(2) nm, ＝98.95(3)°; V＝1.7642(6) nm3; Z＝4; Dc＝1.553 g•cm－3, F(000)＝864, ＝0.126 mm－1. 与其他前体相比, TADNIW更容易经硝解转化为HNIW.

关键词: 四乙酰基二亚硝基六氮杂异伍兹烷, 脱苄, 合成, 晶体结构

Tetraacetyldinitrosohexaazaisowurtzitane (TADNIW•H2O) was synthesized from tetraacetyldi- benzylhexaazaisowurtzitane (TADBIW) by using three inorganic reagents as the nitrosolysis reagents. The molecular structure of purified TADNIW•H2O was determined by 1H NMR, IR, MS spectra and elemental analysis. The single crystal of TADNIW•H2O was prepared from a mixture solvent of ethyl acetate, acetone and DMF. Its structure was testified by X-ray diffraction study. The crystal contains one molecule of TADNIW and one molecule of water, and belongs to monoclinic system with space group P21/n and parameters: a＝1.0738(2) nm, b＝1.4870(3), c＝1.1185(2) nm, ＝98.95(3)°, V＝1.7642(6) nm3, Z＝4, Dc＝1.553 g• cm－3, F(000)＝864, ＝0.126 mm－1. It is easier to prepare HNIW from TADNIW than from any other else precursors with higher yield and purity.

Key words: debenzylation, tetraacetyldinitrosohexaazaisowurtzitane, synthesis, crystal structure