In the present study, heterogeneous Fe-nano-catalyst has been covalently anchored on a modified nanoscale SiO2/Al2O3. The synthesized materials were characterized by FT-IR spectroscopy, DS UV-vis, CHN elemental analysis, BET, EDS, SEM, TEM, TGA and XPS. The catalytic activity of the Fe nano-catalyst (FNC) in the oxidation of ethylbenzene, cyclohexene, and benzylalcohol was studied using tert-butyl hydroperoxide as oxygen source, without the need of any solvent. Oxidation of ethylbenzene, cyclohexene, and benzylalcohol catalyzed by (FNC) gave acetophenone, 2-cyclohexene-1-one and benzaldehyde, respectively, as major products. A suitable reaction condition has been optimized for Fe-nano-catalyst by considering the effect of various parameters such as reaction time and the amount of oxidant, different solvents, concentration of substrate for the maximum conversion of substrates and high selectivity. This catalyst can be easily prepared from inexpensive, commercially available reagent and is stable and reusable for oxidation of ethylbenzene, cyclohexene, and benzylalcohol. (C) 2013 Elsevier B.V. All rights reserved.