3, 4-Bis(pyrazine-2′-y1)furoxan(BPF) was synthesized using self-synthetic 2-chloroximopyrazine as starting material via cyclization reaction. The structure of target compound BPF was characterized by the means of IR, ¹H NMR, ¹³C NMR, elemental analysis and MS. The mechanism of cyclization reaction was investigated. The synthetic conditions of cyclization reactions were optimized. The thermal decomposition mechanism of target compound was studied using a variety of thermal analysis methods just as differential scanning calorimetry(DSC) and thermogravimetric(TG-DTG). Results show that the optimum conditions of cyclizations are that diethyl ether is solvent, 3% Na₂CO₃ aqueous solution is deacidification catalyst, n_actual:n_theory (the amount of Na₂CO₃) is 1.10, reaction temperature is 2-10 ℃, reaction time is 4 h, and the yield of BPF is about 75.6%. The thermal decomposition of target compound BPF is firstly occurred at N—O bond of furoxano ring.