Mixed oxides with perovskite-like structure and the same formal composition La0.6Sr0.4Co0.2Fe0.8O3 (LSCF) were prepared by combustion synthesis and by reactive grinding method. Properties of these materials were compared with properties of a commercially available LSCF mixed oxide. The samples were characterized using XRD, ICP, XPS, TEM, SEM, TPR-H-2, specific surface area (SSA) and acid-base measurements. It was found that although studied materials exhibit similar physicochemical properties they show different catalytic behaviour for phenol alkylation with methanol. Such behaviour can be attributed to differences in surface structure caused by different synthesis route. The main reaction product, i.e. ortho-cresol, was obtained with selectivity higher than 90% (in the whole studied temperature range) at conversion level up to 41% on the material prepared by reactive grinding. (C) 2010 Elsevier B.V. All rights reserved.