3-Amino-4-amidoximinofurazan(AAOF) was synthesized from dicyanopropane by a two-step procedure. By the investigation of reaction parameters on AAOF′s yield,the appropriate reaction conditions listed below: nitrosation temperature 5-10 ℃,oximation temperature 25 ℃,dehydration cyclization temperature 105 ℃ and pH of reaction solution 7-8. The overall yield can be up to 95% and purity 98.5%. The obtained AAOF′s molecular structure was confirmed by IR,¹H NMR,¹³C NMR and elemental analysis. Besides,AAOF was proved to be thermal stable,and its thermal decomposition peak temperature is 203.44 ℃ measured by TG/DTG technique.