Iron containing cubic mesoporous MCM-48 materials were prepared by a modified Stober synthesis method. These materials were characterized by powder X-ray diffraction (XRD). nitrogen isotherms, diffuse-reflectance UV-Vis spectroscopy, and electron microscopy. These materials exhibited high catalytic activity towards the Baeyer-Villiger oxidation of cyclic ketones using benzaldehyde and molecular oxygen. The Fe-MCM-48 mesoporous materials showed excellent recyclability and the integrity of the cubic phase was preserved after the catalytic activity. (C) 2010 Elsevier B.V. All rights reserved.