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Ethanol is currently the biggest liquid biofuel contributor worldwide and it mainly used as source of ethylene and gasoline additive. Should be remarked that ethanol concentration in fuel blend does not exceed 10-15% that caused by a number of its grave disadvantages. One of approach aimed to the catalytic valorization of readily available ethanol into more advanced products e.g. biofuel. Ethanol, a renewable chemical, can be converted to higher molecular weight alcohols, so-called Guerbet alcohols, to be used, for instance, in the production of high-added value linear α-alcohols, e.g. 1 -butanol. It is also well known that butanol can be used as a fuel, having some advantages over ethanol such as a higher energy density (29.2 MJL-1vs. 19.6 MJL-1), lower corrosiveness, and being more suitable for distribution through existing pipelines. Conditions allow high selectivity conversion up to 85-92 % of ethanol into butanol-1, hexanol-1 and octanol-1 were found. Conversion rate of initial ethanol varied from 30 to 70 %. In the first time ever the reaction of β-alkylation of isopropanol with ethanol over heterogeneous catalysts Au-M/Al2O3 was carried out. During combined conversion of ethanol with iso-propanol pentanol-2 was obtained that is structural precursor of valuable monomer - piperylene. Catalysts genesis was investigated with use of XAS, XPS, TEM and EDS. The peculiarities of the reaction mechanism are discussed considering the specific surface and electronic features of the synthesized catalysts.