In the present study, the synthesis of SBA-15 (Santa Barbara Amorphous) support material(SPm) was initially carried out with the method determined according to the literature research. The catalytic property of SBA-15 was imparted by the hydrothermal method (HtM), different from the traditionally applied impregnation method. In this method, the active substance (iron III oxide; Fe2O3) was added to the solution during the synthesis of the SPm. The amount of active substance in the synthesized catalysts was calculated based on the mass ratios of silicon (Si) in SBA-15 and iron (Fe) in Fe2O3. The active substance ratios in the catalysts were determined as 10, 25% Fe/Si. The activities of Fe/SBA-15 catalysts were tested in methyl acetate production (MAP). MAP reaction experiments were carried out in the presence of 0.4g catalyst (Fe/SBA-15), 373K, in autogenous pressure and 2/1 Acetic acid(AA)/methanol(MeOH) feed rate for 48 hours. The effects of active substance loading rate on AA conversion were determined. The structural properties of Fe/SBA-15 catalysts were investigated by XRD, BET, FTIR/DRIFT, SEM/EDX, and MAPPING analysis methods.