In the article the photochemical dissociation of phenol in the participation of TiO2 nano-particles and methyl3-aminocrotonate was done for the first time, the period was taken as 60 minutes, the processing of photochemical dissociation was verified by the curves drawn for reaction solution in the UV radiation “Varian Cary 50” device and the 60% decomposition of phenol was defined. Results confirmed by mass chromatography. The nano-TiO2 were composed of rutile form TiO2 by XRD. The size of nanoparticles was examined by TEM analysis and is about 10-30 nm general surface area of nanoparticles has consisted of 159.6 m2/g. Was carried photochemical degradation of phenol solution under UV irradiation by application of the photocatalytic performance of the synthesized nanoparticles. The phenol degradation was calculated using quantitative analysis, carried out on a 6890N GC-MSD gas chromatograph with an Agilent 5975 high-performance mass-selective detector. Prior to extraction, the pH value of the samples is reduced to pH <4.