Caffeine and coumarin are organic compounds of plant origin, which have biological activity and have found wide application in medicine, pharmaceutical, perfumery and food industries. Recovery of caffeine and coumarin from aqueous solutions using liquid-liquid extraction is the most effective method. In the present work the kinetic dependences of caffeine and coumarin in the aqueous two-phase system (ATPS) of PEG 1500 - Na2SO4 - H2O were experimentally obtained. It was established that equilibrium in the system is achieved after 17 minutes for caffeine and after 12 minutes for coumarin. The effect of ultrasound on the extraction rate of caffeine and coumarin in an aqueous two-phase system was also studied.