Oxidation of toluene (an organic pollutant), into useful chemical products, is of great interest nowadays. However, efficient conversion of toluene under mild and sustainable conditions is a thoughtprovoking task. Here, we report MnMoO 4 nanomaterials (CH1−CH2), synthesized through a very facile solvothermal approach. Catalytic efficiencies of MnMoO 4 nanomaterials were evaluated by direct oxidation of toluene via C−H activation. Toluene was converted into benzaldehyde and benzyl alcohol in the presence of H 2 O 2 as an oxidant at 80 °C. The reaction parameters, that is, catalyst dose, time, and toluene concentration, were varied to obtain the optimal conditions for the oxidation process. The 40.62% maximum toluene conversion rate was obtained after 18 h of oxidation activity with 0.06 g of catalyst CH1. A maximum of 78% benzaldehyde selectivity was obtained with 0.06 g of catalyst CH1 after 18 h of toluene oxidation activity. Also, 62.33% benzyl alcohol selectivity was achieved using 0.1 g of catalyst CH1 after 1 h of activity. Several catalytic cycles were run with CH1 to evaluate catalyst reusability. Potential % toluene conversion was obtained for up to six cycles and their turnover frequencies were found to be 1.94−1.01 s −1 . FTIR spectra of catalyst CH1 before and after recovery indicate no significant change. The good conversion rate of toluene and efficient selectivity toward benzaldehyde and benzyl alcohol indicates the robustness and high potential of these catalysts to oxidize toluene under a milder, greener, and hazardous chlorine-free environment.