3-Cyano-4-nitrofuroxan was synthesized from dicyanopropane via diazotisation, addition, cyclization and oxidation reactions, and its structure was characterized by IR, ¹³C NMR and ¹⁵N NMR and elemental analysis. The yields of cyclization and oxidation reactions are 55.1% and 83.6%, respectively. In the ¹³C NMR, the chemical shifts were assigned by comparing with 3-cyano-4-nitrofurazan, which further confirm the configuration of 3-cyano-4-nitrofuroxan. The bond order, density, enthalpy of formation and detonation parameters of 3-cyano-4-nitrofuroxan were calculated theoretically. Results show that the minimum bond order are N(1)—O(4)(0.84) and C(6)—N(9) (0.91), the density is up to 1.74 g·cm^-3, the enthalpy of formation is 352.6 kJ·mol^-1, and the detonation velocity and detonation pressure are 8352 m·s^-1 and 30.9 GPa, respectively.