3,4⁃双((4⁃氯⁃3,5⁃二硝基⁃1H⁃吡唑⁃1⁃基)甲基)‐氧化呋咱的合成、表征与晶体结构

Synthesis,Characterization and Crystal structure of 3,4⁃Bis((4⁃chloro⁃3,5⁃dinitro⁃1H⁃pyrazol⁃1⁃yl)methyl)⁃furoxan

以4-氯吡唑为原料,设计并合成了一种新的含能化合物——3,4-双((4-氯-3,5-二硝基-1H-吡唑-1-基)甲基)-氧化呋咱,通过溶剂蒸发获得到了晶体。通过核磁共振、傅里叶红外光谱、差示扫描量热仪和热失重分析仪对该化合物及其中间产物的结构进行了表征,并通过X射线单晶体衍射仪对产物晶体结构进行了测试。测试结果显示,该化合物属于正交晶空间群Pbca,晶胞参数为a=10.1817(7)Å,b=16.1917(11)Å,c=21.7300(16)Å,V=3582.4(4)Å^(3),α=90°,β=90°,γ=90°,Z=8,Dc=1.836 g·cm^(-3)。采用Kamlet-Jacobs半经验方程预测了化合物的爆速8304 m·s^(-1)和爆压30.5 GPa。采用BAM标准方法进行感度测定,测得撞击感度为9 J,摩擦感度为180 N。

A new high-energy compound 3,4-bis((4-chloro-3,5-dinitro-1H-pyrazol-1-yl)methyl)-furoxan was synthesized by using 4-chloropyrazole as raw material,and its single crystal was obtained by solvent evaporation.The structures of this compound and its intermediates were characterized by 1H and 13C NMR,FT-IR,DSC and TG,and the crystal structure of the product was characterized by X-ray single crystal diffraction.Results show that the compound belongs to the orthorhombic space group Pbca,a=10.1817(7)Å,b=16.1917(11)Å,c=21.7300(16)Å,V=3582.4(4)Å^(3),α=90°,β=90°,γ=90°,Z=8,Dc=1.836 g·cm^(-1).The Kamlet-Jacobs semi-empirical equation was used to predict the explosion velocity of 8304 m·s^(-1) and the explosion pressure of 30.5 GPa.The sensitivities of this compound were measured by the BAM standard method,and the measured impact sensitivity is 9 J and the friction sensitivity is 180 N.