4,4′,6,6′-Tetra(azido)azo-1,3,5-triazine(TAAT) was synthesized with cyanuric chloride and hydrazine hydrate as primary materials. This synthesis is a four-step process including coupling,hydrazinolysis,diazotization and oxidation in turn. Each reaction process,especially the oxidizing reaction is described in details. The investigation indicates that chlorine can transform 94% 4,4′,6,6′-tetra(azido)hydrazo-1,3,5-triazine into TAAT but N-bromosuccinimide just transforms 84%. The DSC,IR,NMR and elemental analysis determine the structure of TAAT and its intermediates. The characterization of DSC shows TAAT decomposes at 198 ℃. A free radical mechanism is presented to interpret the oxidizing reaction.