The effect of calcination conditions on MoO3/SiO2 catalysts for the synthesis of methylphenyl carbonate was investigated in terms of catalytic activities and surface properties. The calcination temperature was varied in the range of 300 to 800degreesC. These calcination conditions have shown a close relationship with the catalyst activities. The optimal calcination temperature of MoO3/SiO2 was found to be around 550-600degreesC. The catalysts were characterized by XRD, SEM, Fr-IR and XPS analysis.