SiO 2 nanoparticles modi¯ed with aminopropyl-triethoxysilane (APTES) were used as hard templates for preparing porous MoS 2 . The method o®ers the advantages of simple steps, convenient operation, controllable pore size, and a speci¯c surface area. Two morphologies of MoS 2 were obtained by using thiourea and L-cysteine as sulfur sources, respectively. Porous MoS 2 prepared by using thiourea had a smooth surface, whereas the surface of porous MoS 2 prepared with L-cysteine had many burrs. The MoS 2 nanomaterials with the respective morphologies were used to catalyze the hydrodeoxygenation (HDO) reaction. The activity of MoS 2 prepared with L-cysteine was lower than that prepared with thiourea. Transmission electron microscopy and X-ray di®raction analyses showed that MoS 2 had a large sheet-shaped structure and high crystallinity, leading to high reaction activity and high selectivity for cyclohexane. The reaction temperature also in°u-enced the HDO signi¯cantly. The mechanism of hydrogenation of phenol was discussed.