A new method to synthesize 3, 3′-diamino-4, 4′-azoxyfurazan (DAOAF) which used 3, 4-diaminofurazan as raw material and 3-amino-4-formylaminofurazan or 3, 4-diformylaminofurazan as intermediate was introduced. 3-amino-4-formylaminofurazan or 3, 4-diformylaminofurazan was oxygenating by 30% H₂O₂ in solvent of 1, 4-dioxane. After refluxing for 4 h, DAOAF was obtainded with yield 97% or 89%. The product was characterized by ¹H NMR, ¹³C NMR, IR and EI.