The influence of iron oxide supported on zinc aluminate on catalytic activity and physicochemical properties of the samples was investigated. Zinc aluminate was prepared by coprecipitation followed by hydrothermal treatment at elevated temperatures and iron as Fe(NO3)3 was supported on ZnAl2O4 by wet impregnation method. The obtained samples were characterized by X-ray diffraction, textural measurements (SBET, Vp, pore size distribution), and temperature programmed reduction (TPR-H2). Activities and selectivities obtained in the catalytic alkylation of phenol and anisole with methanol, performed in the presence of ZnAl2O4 and 8%Fe2O3/ZnAl2O4, were studied and compared. Experimental data show that the addition of Fe2O3 into ZnAl2O4 does improve the selectivity of alkylation. As a result of phenol methylation there were obtained its ort/zo-derivatives (ortho-creso\ and 2,6-xylenol) over ZnAl2O4 and 8%Fe2O3/ZnAl2O4 with selectivities 54.9 and 61.5%, respectively. The application of anisole as raw material in studied reaction of methylation led to obtain of 2,3,5-trimethylphenol with 76.5% selectivity at 342°C K in the presence of 8%Fe2O3/ZnAl2O4.