Chromium substituted cobalt ferrospinels were prepared by soft citrate gel method. The synthesized material was characterized by various physico-chemical methods. All the samples showed a single-phase cubic structure. Lattice constant varies from 8.389 to 8.323 Å . Transmission electron microscopic study indicated the nanostructure of the catalysts while homogenous grain distribution was presented by scanning electron microscopic studies. The catalytic activity of the samples was investigated towards acetylation of phenols. The presence of active centers on the surface of the material was confirmed through pyridine adsorption studies. The surface acidity of the catalyst is responsible for better catalytic performance. The material was found to serve as a promising catalyst for acylation and benzoylation of phenols under solvent free condition. These catalysts are∼100% selective towards o-acylation of phenols, a promising reaction for perfumery intermediates. The catalysts were seen to be reusable without any further treatment. Catalytic activities of cobalt, chromium and iron oxides were also investigated for comparison. The cobalt ferrospinel was found to have better catalytic activity as compared to the Cr substituted ferrospinels and the pure oxides. Cobalt ferrite catalyst offers high yields in a short reaction time under solvent-free conditions.