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有机化学 ›› 2010, Vol. 30 ›› Issue (07): 1044-1050. 上一篇    下一篇

研究论文

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

周彦水，王伯周*，周诚，李建康，陈智群，廉鹏，张志忠   

  1. (西安近代化学研究所 西安 710065)
  • 收稿日期:2009-08-19 修回日期:2010-01-28 发布日期:2010-02-23
  • 通讯作者: 王伯周 E-mail:wbz600@163.com
  • 基金资助:

    国防基础研究资助项目

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

ZHOU Yan-Shui, WANG Bo-Zhou, ZHOU Cheng, LI Jian-Kang, CHEN Zhi-Qun, LIAN Peng, ZHANG Zhi-Zhong   

  1. (Xi an Modern Chemistry Research Institute, Xi an 710065)
  • Received:2009-08-19 Revised:2010-01-28 Published:2010-02-23

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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) nm, Z＝4, D＝1.743 g/cm, μ＝0.150 mm, 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% (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

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, H NMR, C NMR, N 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 parameters 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) nm, Z＝4, D＝1.743 g/cm, μ＝0.150 mm, 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).

Key words: 3,4-bis(4 -azidofurazano-3 -yl)furoxan, DAZTF, synthesis, characterization, crystal structure