Synthesis, Thermal Behaviours and Crystal Structure of 1,1',-Dioxide-7,7,-bis(terfurazan[3,4-b:3,4'-d:3',4'-f]azepine)

摘要

1'1'-Dioxide-7,7'-bis(terfurazan[3,4-b:3,4'-d;3",4"-f|azepine) was synthesized from 3,4-te(4-nitrofurazan-3-yl)furoxan by cyclization and nitration with a yield of 25.7 % and its structure and intermediate were characterized by 'H NMR,' 'C NMR, FT-1R and elementary analvsis. Its single crystal was obtained and its crystal structure was studied by X-ray single-crystal diffraction analysis. The title compound (C_(18) H_(13)N_(14)O_(10), M, = 584.42) crystallizes in trigonal system, P3(2) space group and constituted one l,l'-dioxide-7.7'-te (terfurazan{3,4-d:3,4':3",4"-f|azepine) and two acetone molecules, with a =15.460 (18), b = 15.460 (18), c = 9.603 (11) A, V = 1988 (4) A~3. Z = 3. Dc-1.465 g/cm~3 λ = 0.071073 A, u(MoKa) = 0.123 mm~(-1), F(000) = 894, S = 1.022, R = 0.0720 and wR = 0.1838. In DSC and TG-DTG techniques suggest that there are two main decomposition peaks at 288.7 and 338.7 °C. The results show that the title compound had favorable thermal stability.