Synthesis of a series of Ti loaded MCM‐48 mesoporous materials have been reported. The formation of these materials with incorporated titanium into the mesoporous framework was confirmed using various characterization techniques. The catalytic activity of the synthesized materials was investigated for the selective oxidation of aniline to azoxybenzene in presence of H2O2 as the oxidant. Variety of substituted anilines gave the corresponding product in good yield under the optimized reaction condition. Reusability of the catalyst was also demonstrated upto 4th run with minimal loss in catalytic activity.