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

摘要

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℃.%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。