MoO(3)/SiO(2) composite with varying amounts of MoO(3) 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 NH(3)-TPD. The activities of synthesized MoO(3)/SiO(2) 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) /ZrO(2)). Under the similar reaction conditions, synthesized 10 wt.% MoO(3)/SiO(2) catalyst calcined at 500 C was found to be the most active in the condensation of anisole with paraformaldehyde.