3,4-Bis(3′-nitrophenyl-1′-yl)furoxan was synthesized by two methods (oxidative dehydrogenation reaction and dimerization reaction of nitrile oxide). The target compound was characterized by IR, NMR, elemental analysis and DSC. The target compound was obtained with yield of 32.4% by the oxidative dehydrogenation reaction which involved nitration of benzil, hydroamine addition,and oxidative cyclization,and the target compound was obtained with yield of 21.0% by the dimerization reaction of nitrile oxide which involved hydroamine addition of benzonitrile, diazotization,intermolecular cyclization and nitration of 3,4-bisphenyl furoxan. DSC curve shows that the exothermic peak of the opening-ring for 3,4-bis(3′-nitrophenyl-1′-yl)furoxan is 280.7 ℃ with releasing heat of 1142 J·g^-1.