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Abstract: High surface area and high dispersion Mo/MCM-41 catalysts were successfully prepared using high-purity silatrane and molybdenum glycolate precursors. The precursors were synthesized using the Oxide One Pot Synthesis (OOPS) process. Mo was loaded onto MCM-41 by impregnation before and after heat treatment. After heat treatment, the catalysts were characterized using DRUV, XRD, FTIR, Laser Raman and BET. The %Mo dispersion was as high as 10 mol% or 0.265 g MoO3/g SiO2 while the structure of MCM-41 was still retained. Bulk MoO3 was observed in the case of Mo-loaded onto the calcined support of MCM-41(c). The Mo-loaded uncalcined silicate MCM-41 support showed better catalytic activity during the peroxidative reaction. [Copyright &y& Elsevier]