3,3′-Diamino-4,4′-azofuroxan (DAAFO) was synthesized by a two-step process,with 4-amino-3-azidocarbonylfuroxan as precursor which was synthesized by a three-step process with ethyl acetoacetate as starting material. The DAAFO and mediate products were characterized by DSC-TG,elemental analysis,IR and MS. And the sensitivity and DSC analysis of DAAFO were carried out and compared. The results show that 4-amino-3-azidocarbonylfuroxan is more sensitive than diaminofurazan and HMX. The peak decomposition temperature of DAAFO is 208.17 ℃,lower than that of 3,3′-diamino-4,4′-azofurazan (DAAF) and 3,3′-diamino-4,4′-azoxyfurazan (DAOAF).