3,4-Diphenylfuroxan and four no-reported compounds 3,4-bis(pyridine-2′-yl)furoxan, 3,4-bis(pyridine-3′-yl)furoxan, 3,4-bis(pyridine-4′-yl)furoxan and 3,4-bis(pyrazine-2′-yl)furoxan were self-designed and synthesized using chloride oxime-based compounds as starting materials and the synthetic method of dimerization reaction of cyanide oxidation. The structures of target compounds were characterized by IR, NMR, MS and elemental analysis. The effects of different substituents, different catalysts,reaction temperature on the synthesis of furoxan derivatives using dimerization reaction were preliminarily investigated. Results show that the electron withdrawing ability of substituents is stronger,the structure of cyanide oxidation is more easily generated,and the yields of target products are higher. The inorganic weak base(for example Na2CO3, KHCO3) is usually chosen as catalyst. The reaction temperature is usually controlled at 2-10 ℃. Under the optimal conditions, the yields of target compounds are 64.7%, 71.3%, 70.0%, 71.1% and 75.6%, respectively.