A one-pot method was used to synthesize vinyl-functionalized mesoporous silica with highly dispersed gold nanoparticles. Samples were characterized using physical adsorption of nitrogen, X-ray diffraction, transmission electronic microscope, solid-state nuclear magnetic resonance, X-ray photoelectron spectrometer, and ultraviolet-visible spectrometer. It was found that Au was anchored on the vinyl functionality as highly dispersed and uniform nanoparticles. Catalytic results showed that such Au nanoparticles displayed very high catalytic activity and selectivity in solvent-free selective oxidation of cyclohexane with molecular oxygen. (C) 2010 Elsevier B.V. All rights reserved.