Nanostructured (I) Fe(2)O(3) and Co(3)O(4) stabilized in the mesopores of an MCM-41 sieve and immobilized (II) FeCl(2), Fe(acac)(3), and FePc on the surface of an MCM-41 sieve functionalized with 3-aminopropyltriethoxysilane (3-APTES) were synthesized and examined. The materials were characterized by elemental analysis, H(2) -TPR, X-ray diffraction analysis, IR and electronic absorption spectroscopy, as well as by low-temperature N(2) adsorption. The catalytic activity was evaluated in the reaction of liquid-phase oxidation of benzene and phenol with hydrogen peroxide. Catalysts I showed a low activity in benzene oxidation, whereas catalysts II were active in the oxidation of phenol.