Various mesoporous silica supported Pd materials were prepared by different methodologies in order to control and optimize the metal nanoparticle sizes for catalytic applications. The catalytic activities (conversion, mol% and selectivity to methyl-cinnamate) of the supported palladium catalysts were investigated in the Heck reaction under microwave irradiation using various haloarenes. Pd materials prepared by co-precipitation exhibited a very poor activity in the Heck reaction compared to that of Pd impregnated samples. Impregnated materials prepared without the use of a specific reducing agent had comparable activities to those of APTS-NaBH4 reduced Pd materials, validating the simplicity of the methodology. High selectivities to methylcinnamate were obtained for all materials.