In this paper we elected to nitrate p-xylene because this compound has onlyone mononitro- and trinitro- isomer. Trinitro-p-xylene was used as a starting material forthe synthesis of other compounds in subsequent work. The mononitration of p-xylene canbe easily carried out at 30°C. Nitro-p-xylene is easily nitrated to dinitro-p-xylene at atemperature of 80°C. The trinitro-p-xylene can be obtained at 120°C. Single crystals of2,3-dinitro-p-xylene and 2,3,5-trinitro-p-xylene were grown using theslow cooling method and we report the X-ray structure of the former. The thermaldecomposition of the compounds was studied using differential scanning calorimetry(DSC) and thermogravimetry-derivative thermogravimetry (TG-DTG) techniques andFT-IR. The target compounds were also characterized by 1H-NMR, 13C-NMR and MS.