In this study, for the first time, nitroalkanes, especially nitromethane, have been used as electron acceptors for the highly chemoselective oxidation of alcohols in the presence of a TiO₂ photocatalyst under 400 nm LED irradiation. The reactions showed excellent selectivity for the production of aldehydes. Interestingly, aldehydes such as benzaldehyde and p-methoxybenzaldehyde are stable under the reaction conditions. In the case of the use of 2-nitropropane and 2-methyl-2-nitropropane, the product imine, which is the result of the reaction of the aldehyde with aliphatic amine, is also obtained.