Fe-MCM-41 has been characterized in detail and studied for epoxidation of alkenes with H2O2. UV-vis, ESR, Fe K-edge XAFS and UV-Raman spectroscopic studies suggest that iron in Fe-MCM-41 is highly dispersed and mainly incorporated into the framework of MCM-41. Fe-MCM-41 is effective for epoxidation of alkenes including styrene, cyclohexene and many other cyclic alkenes with H2O2. The tetrahedrally coordinated iron sites in the framework of MCM-41 are probably responsible for the epoxidation reactions.