Sn-containing hydrotalcite-like compounds were prepared by three different methods such as (i) direct synthesis, (ii) ion-exchange and (iii) grafting. These catalysts were proved to have framework Sn species by powder X-ray diffraction (XRD) analysis and UV-vis spectroscopy. The catalysts prepared by three methods were found to be active and selective for the liquid phase Baeyer–Villiger (BV) oxidation of admantonone using hydrogen peroxide (H2O2) as an oxidant and acetonitrile as a solvent. The Sn-hydrotalcite-like catalysts prepared by ion-exchange method exhibited better catalytic performance than the catalysts prepared by other two methods. Among the ion-exchanged hydrotalacite-like catalysts, 3% Sn ion-exchanged hydrotalcite exhibited superior activity at 30% conversion and 100% selectivity.