For the first time, there was carried out photochemical dissociation of phenol in the presence of TiO 2 nanoparticles and methyl-3-aminocrotonate. It is established that 80% of phenol was decomposed. The process lasted for two hours. Results are confirmed by the mass-chromatography. The nanocrystalline TiO 2 powders were composed of rutile form TiO 2 obtained by XRD. The size of nanoparticles was examined by transmission electron microscopy analysis and is about 10-20 nm, general surface area of nanoparticles made up 159.6 m 2 /g. The photolysis process was carried out at UV radiation and the coefficient dependence on the wavelength was determined by the "Varian" device.