The present invention belongs to the synthetic preparation of 3,5-dimethyl-4-nitropyridine-N-oxide. The method comprises in a two steps. First step is oxidation of 3,5-Dimethyl pyridine by using hydrogen peroxide. Adding a catalyst in the first step is reduces the quantity of acetic acid which is very useful during the scale up. It reduces waste generation. The second step is nitration by using sulfuric acid and nitric acid. The synthesis method of the 3, 5-dimethyl-4-nitropyridine-N-oxide carried out without isolation of 3, 5-Dimethyl pyridine N-Oxide. It reduces the organic waste as well as improves the reaction yield. The final compound was characterized by NMR, Mass spectra and elemental analysis.