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7H-三呋咱并[3,4-b:3′,4′-f:3″,4″-d]氮杂环庚烯合成、晶体结构及热行为研究
Synthesis, Crystal Structure and Thermal Behavior of 7H-trifurazano[3,4-b:3′,4′-f:3″,4″-d]azepine
【Author】 JIA Siyuan;WANG Bozhou;ZHANG Haihao;LAI Weipeng;ZHOU Cheng;Xi’an Modern Chemistry Research Institute;
【机构】 西安近代化学研究所;
【摘要】 以3,4-双(3′-氨基呋咱-4′-基)呋咱(BATF)为原料,设计了新型含能材料7H-三呋咱并[3,4-b:3′,4′-f:3″,4″-d]氮杂环庚烯(HTFAZ)的合成路线,经氧化和环化2步反应合成了HTFAZ,产率50.2%,并采用红外光谱、核磁共振、元素分析和质谱等进行了结构表征。培养了HTFAZ单晶,X射线单晶衍射分析结果表明:HTFAZ晶体结构属单斜晶系,空间群为P2(1)/n,a=7.252(15)nm,b=6.458(14)nm,c=16.814(4)nm,V=778.1(3)3,Z=4,Dc=1.871 g/cm3,F(000)=440,R1=0.0353,wR2=0.0895。采用DSC和TG-DTG研究了ATFAZ的热分解过程,在10℃/min的升温条件下,其熔点为193.1℃,在200~295℃之间具有明显的挥发现象。
【Abstract】 Using 3,4-bis(3′-nitrofurazan-4′-yl) furazan(BATF) as starting material, an energetic material 7-aminotrifurazano[3,4-b:3′,4′-f:3″,4″-d]azepine(HTFAZ)was synthesized by a designed synthetic routes of oxidation and cyclization with a total yield of 50.2%,and its structure was characterized by NMR, IR, MS, elemental analysis and single crystal X-ray diffraction. The single crystal of HTFAZ was studied by X-ray single crystal diffraction in the first time, and followed as: Its crystal belongs to orthorhombic, space group is P2(1)/n with a=7.252(15) nm,b=6.458(14)nm,c=16.814(4)nm,V=778.1(3) 3, Z=4,Dc=1.871 g/cm3,F(000)=440,R1= 0.0353 and wR2=0.0895. The thermal behavior of HTFAZ was studied by DSC and TG – DTG and followed as: its melting point was 193.1℃ at the rate of 10℃/min, the main thermolysis process was produced in range of 200~295℃.
【Key words】 organic chemistry; 7-aminotrifurazano[3; 4-b′; 4′-f″; 4″-d]azepine; synthesis; crystal structure; thermal behavior;
- 【会议录名称】 第十六届中国科协年会——分9含能材料及绿色民爆产业发展论坛论文集
- 【会议名称】第十六届中国科协年会——分9含能材料及绿色民爆产业发展论坛
- 【会议时间】2014-05-24
- 【会议地点】中国云南昆明
- 【分类号】TQ560.1
- 【主办单位】中国科学技术协会、云南省人民政府