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Novel organic‐inorganic hybrid mesoporous materials containing diimine moieties inside the pore wall were used for the grafting of an oxo‐vanadium Schiff base complex at the mesopore surface. The prepared catalyst was found to be highly active and selective for the oxidation of a variety of primary, secondary and α‐hydroxy carbonyl compounds to the corresponding aldehydes, ketones and 1,2‐dicarbonyl compounds using tert‐butyl hydroperoxide as oxidant under mild reaction conditions. After completion of the reaction, the catalyst could easily be recovered by simple filtration and could be reused several times without significant change in the catalytic efficiency. Importantly, the catalyst did not show any leaching during the reaction, confirming that the prepared catalyst was truly heterogeneous in nature.