3,4-双(4'-叠氮基呋咱-3'-基)氧化呋咱合成、表征与晶体结构研究  

Synthesis, Characterization and Crystal Structure Study on 3,4-Bis(4'-azidofurazano-3'-yl)furoxan

作　　者：周彦水[1] 王伯周[1] 周诚[1] 李建康[1] 陈智群[1] 廉鹏[1] 张志忠[1] 

机构地区：[1]西安近代化学研究所,西安710065

出　　处：《有机化学》2010年第7期1044-1050,共7页Chinese Journal of Organic Chemistry

基　　金：国家自然科学基金(No.2371000415)资助项目

摘　　要：自行设计了3,4-双(4'-叠氮基呋咱-3'-基)氧化呋咱(DAZTF)的分子结构与合成方法,采用3-氨基呋咱-4-酰氯肟为原料,经重氮化、叠氮化、分子间缩合环化等反应合成目标化合物DAZTF,总收率为81%,并采用红外光谱、核磁共振光谱、质谱以及元素分析等进行了结构表征;首次培养了DAZTF单晶,X射线单晶衍射结果表明:DAZTF晶体属于单斜晶系,P2(1)/n空间群,a=1.1620(6)nm,b=0.6977(4)nm,c=1.4446(8)nm,α=90o,β=98.331(9)o,γ=90o,V=1.1589(11)nm3,Z=4,Dc=1.743g/cm3,μ=0.150mm-1,F(000)=608;同时,开展了DAZTF部分性能研究,其熔点50～52℃,分解温度204.20℃,摩擦感度86%～100%(90°摆角),撞击感度86%～100%(10kg,25cm).3,4-Bis（4＇-azidofurazano-3＇-yl）furoxan （DAZTF）, a novel energetic material, was devised for the first time and synthesized from 3-aminofurazan-4-carboxchloridoxime by the process of diazotization, azidation and dimerization in a yield of 81%, and its structure was confirmed by IR, 1H NMR, 13C NMR, 15N NMR, MS and elemental analysis. The single crystal of DAZTF was cultivated and tested by X-ray single-crystal diffraction. The crystal belongs to monoclinic system, space group P2（1）/n with crystal parame-ters a=1.1620（6） nm, b=0.6977（4） nm, c=1.4446（8） nm, α=90°, β=98.331（9）°, γ=90°, V=1.1589（11） nm3, Z=4, Dc=1.743 g/cm3, μ=0.150 mm-1, F（000）=608, and the final deviation factor R is 0.038. The part experimental properties of DAZTF had been obtained which m.p. was 50～52 ℃, temperature of decomposition was 204.20 ℃ （DSC）, friction sensitivity was 86%～100% （90°） and impact sensitivity was 86%～100% （10 kg, 25 cm）.

关 键 词：3 4-双(4'-叠氮基呋咱-3'-基)氧化呋咱 DAZTF 合成 表征 晶体结构 

分 类 号：O626.1[理学—有机化学]