Tris(para-nitrophenyloxymethyl)nitromethane was synthesized via reaction, esterification and substitution reaction using nitromethane as starting material. The structures of intermediate compounds and title compound were confirmed by ¹H NMR and IR. Thermal behavior of the title compound was determined by TG-DSC. Results show that the optimized conditions of substitution reaction are: reagent ratio 1:3.5, reaction temperature 120 ℃, reaction time 24 h, potassium carbonate as acid binding agent. The total yield is 51.2%. The melting point and thermal decomposition temperatures of the title compound are 186.94 ℃ and 340.59 ℃ respectively. The total mass loss in the temperature ranges 246.2-499.3 ℃ is 62%. The title compound does not decompose completely at 500 ℃, showing that the title compound has a good thermal stability.