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7-氨基三呋咱并[3,4-b:3′,4′-f:3″,4″-d]氮杂环庚烯的合成、晶体结构及热行为 被引量:3

Synthesis,Crystal Structure and Thermal Behavior of 7-Aminotrifurazano[3,4-b:3′,4′-f:3″,4″-d]azepine
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摘要 以3,4-双(3′-氨基呋咱-4′-基)呋咱为原料,经氧化和环化2步反应合成了7-氨基三呋咱并[3,4-b:3′,4′-f:3″,4″-d]氮杂环庚烯(ATFAZ),收率66%;用红外光谱、核磁共振、元素分析和质谱对其结构进行了表征,用 DSC和 TG-DTG 研究了 ATFAZ 的热分解过程;培养了 ATFAZ 单晶,用 X-射线单晶衍射对晶体结构进行分析。结果表明,ATFAZ 晶体属正交晶系,空间群为 Pbca,a =1.273 nm,b =0.876(3)nm,c =1.560(6)nm,V =1.740(11) nm3,Z =8,Dc =1.788 g·cm-3,μ=0.141 mm-1,F(000)=944,R 1=0.0338,wR 2=0.0976。在10℃/min 的升温条件下,其熔点为204~207℃,在210~282℃具有明显的挥发现象。 Using 3,4-bis (3′-aminofurazan -4′-yl)furazan as starting material,an energetic material 7-aminotri-furazano[3,4-b:3′,4′-f:3″,4″-d]azepine(ATFAZ)was synthesized through oxidation and cyclization with a total yield of 66%,and its structure was characterized by IR,13 C NMR,elemental analysis and MS.The thermal behavior of ATFAZ was studied by DSC and TG-DTG.The single crystal of ATFAZ was cultured and analyzed by X-ray single crystal diffraction.The results show that the crystal of ATFAZ belongs to orthorhombic,space group is Pbca with a=1 .273(5)nm,b=0.876(3)nm,c =1.560(6)nm,V =1 .740(11 )nm3 ,Z =8,Dc =1 .788 g·cm-3 ,μ=0.141 mm-1 ,F(000)=944,R 1 = 0.033 8 and wR 2 =0.097 6.Its melting point was 204 -207℃ at the heating rate of 10 ℃·min-1 ,and the main thermolysis process occurred in the range of 210-282℃.
出处 《火炸药学报》 EI CAS CSCD 北大核心 2014年第4期19-24,共6页 Chinese Journal of Explosives & Propellants
基金 总装"十二五"预研项目(NO.51328050205)
关键词 有机化学 7-氨基三呋咱并[3 4-b 3′ 4′-f 3″ 4″-d]氮杂环庚烯 ATFAZ 晶体结构 热行为 organic chemistry 7-aminotrifurazano [3,4-b:3′,4′-f:3″,4″-d]azepine ATFAZ crystal structure thermal behavior
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