四乙酰基二亚硝基六氮杂异伍兹烷水合物(TADNIW·H_2O)的合成与晶体结构  

Synthesis and Crystal Strucutre of Tetraacetyldinitroso-hexaazaisowurtzitane (TADNIW·H_2O)

作　　者：吕连营[1] 欧育湘[2] 王建龙[3] 

机构地区：[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

出　　处：《有机化学》2005年第4期399-404,共6页Chinese Journal of Organic Chemistry

基　　金：国防科工委预研基金(No.12060451867)资助项目.

摘　　要：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1HNMR,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,β=98.95(3)°;V=1.7642(6)nm3;Z=4;Dc=1.553g?cm-3,F(000)=864,μ=0.126mm-1.与其他前体相比,TADNIW更容易经硝解转化为HNIW.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 TAD-NIW 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, β=98.95(3)°, V=1.7642(6) nm3, Z=4, Dc=1.553 g? cm-3, F(000)=864, μ=0.126 mm-1. It is easier to prepare HNIW from TADNIW than from any other else precursors with higher yield and purity.

关 键 词：晶体结构 亚硝基 四乙酰基二苄基六氮杂异伍兹烷 合成 六硝基六氮杂异伍兹烷 水合物 高能量密度化合物 精细化工产品 X射线衍射法 三元复合 无机试剂 分子结构 乙酸乙酯 结构鉴定 元素分析 混合溶剂 单斜晶系 晶胞参数 

分 类 号：O626[理学—有机化学]