5-Amino 3-nitro-1,2,4-triazole (ANTA) as well as its intermediate was synthesized from 3,5- diamino-1,2,4-triazole after diazotization, neutralization and reduction. Its structure was characterized by IR, MS, ¹H NMR and elemental analysis. In addition, the effects of reaction temperature on yield and purity were investigated. The synthetic procedures of ANTA were optimized with the overall yield to be 64%, and purity to be 98%.