The high energy compounds bis[4-nitraminofurazanyl-3-azoxy]azofurazan (ADNAAF) was synthesized from bis[4-aminofurazanyl-3-azoxy]azofurazan (ADAAF) using glyoxal as starting material. The structures of ADNAAF and ADAAF were characterized by IR, NMR and MS. With KBrO₃ and glacial acetic acid as oxidation system, the factors affecting the synthesis of ADAAF were studied. The optimum reaction conditions were found to be as follows: the reaction temperature 50 ℃, reaction time 16 h, andn(CH₃COOH) : n(DAOAF)=68:1, with a yield of 58.5%. The thermal properties of ANDAAF and ADAAF were studied by differential scanning calorimetry and thermogravimetry analysis. Results show that the initial decomposition temperature of ADAAF and ADNAAF are 267.18 ℃ and 114.81 ℃, respectively, and the mass loss of ADAAF due to overall reaction (50-500 ℃) is 90.91% and ADNAAF (70-500 ℃) is 100%. The detonation performances of ADNAAF were estimated by Gaussian 03. The detonation velocity of ADNAAF is 9140 m·s^-3 and detonation pressure is 38 GPa, which indicates that ADNAAF is a high energy density compound with potential application value.