The gas-phase catalytic transformations of anisole on two catalytic systems: ZnAl2O4 (A) and 8%Fe2O3/ZnAl2O4 (B) have been studied. Catalyst A was synthesised at hydrothermal conditions from Zn and Al nitrates; catalyst B was made from catalyst A by additionally impregnating with aqueous solution of ferric nitrate. Experimental data show that the addition of iron oxide (Fe2O3) into zinc aluminate improves the catalytic activity i.e. anisole conversion and total ortho-selectivity to ortho-cresol and 2,6-xylenol. On the surface of both catalysts, Lewis acid sites are present. Catalyst A is characterised by higher concentration of Lewis acidity. The proposal of the reaction mechanism in the presence of catalysts was presented. (C) 2004 Elsevier B.V. All rights reserved.