MoO3/SiO2 composite with varying amounts of MoO3 loading (1-20 wt.%) were prepared by sol-gel method and calcined at 500 C. These catalysts were employed for the liquid phase condensation of anisole with paraformaldehyde. All the catalysts were characterized by N-2 sorption, XRD, and NH3-TPD. The activities of synthesized MoO3/SiO2 catalysts were compared with p-toluene sulfonic acid (p-TSA), the most frequently used catalyst for the condensation reactions, and with a supported metal oxide (WO (x) /ZrO2). Under the similar reaction conditions, synthesized 10 wt.% MoO3/SiO2 catalyst calcined at 500 C was found to be the most active in the condensation of anisole with paraformaldehyde.