[en] Two new interesting compounds, ethanedial-1,2-bis-(2-(1-amino-2,2-dinitroethenyl))hydrazone (EDNH) and 3-dinitromethyl-1,2,4-triazine (DNTA), were synthesized by the reaction of 1-amino-1-hydrazino-2,2-dinitroethylene (AHDNE) and glyoxal under different acid–base conditions, and reaction processes were discussed. Thermal decomposition behaviors of the two compounds were studied with DSC and TG/DTG methods, and the kinetic equations of decomposition process were obtained. Self-accelerating decomposition temperature and critical temperature of thermal explosion are 193.92 and 209.75 °C for EDNH, and 242.46 and 259.94 °C for DNTA, respectively. Specific heat capacities of the two compounds all present a square relationship with temperature in determined temperature range, and molar heat capacities at 298.15 K are 331.30 and 213.13 J mol⁻¹ K⁻¹, respectively. DNTA and EDNH are relatively insensitive (> 35 and > 25 J), which are much lower than that of AHDNE.