Abstract A high energetic compound 4‐diazo‐2,6‐dinitrophenol was synthesized by employing one‐pot facile method from 4‐chloro‐3,5‐dinitroaniline. Its structure was characterized by Fourier transform infrared spectroscopy (FT‐IR), elemental analysis (EA), and nuclear magnetic resonance spectroscopy ( 1 H NMR, 13 C NMR and 15 N NMR). The crystal structure was determined using an X‐ray single crystal diffractometer. The detonation properties of 4‐diazo‐2,6‐dinitrophenol and 6‐diazo‐3,5‐dichloro‐2,4‐dinitrophenol were compared by using Kamlet formula. Besides, the thermal behavior of 4‐diazo‐2,6‐dinitrophenol was analyzed by differential scanning calorimetry (DSC) and accelerating rate calorimeter (ARC), then according to the thermal analysis data, the thermal decomposition kinetics parameters were calculated using the thermal analysis data based on Kissinger method and Flynn‐Wall‐Ozawa method.