The paper presents experimental data on synthesis of the substituted 2,3-dialkylquinolines by the condensation reaction of aniline with photooxidation products of aliphatic alcohols (C₂-C₅). The synthesis is a 2-stage process. The first stage is the photo-oxidation of alcohols to aldehydes using FeCl₃∙6H₂O under UV irradiation. The second stage is the condensation of aniline with aldehydes photosynthesized under the effect of the catalyst FeCl₃∙6H₂O. The influence of nature of the solvent, pH and the ratio of initial components on the yield of 2,3-dialkylquinolines are investigated.