Phenol is a highly toxic chemical tohumansand aquatic biodiversity. The desirable limit according to [Bureau of Indian Standards] for phenol in drinking water is 0.001 mg/L. Several industries and anthropogenic activities are responsible for entry of organic compounds in natural water resources. The study was carried out for the removal of phenol present in the wastewater by liquid-liquid extraction process. In this process toluene is used in capacity of solvent to extract phenol from wastewater. Chemical oxygen demand of wastewater was determined before and after extraction, to check the efficiency of treatment. The laboratory experiments were carried out on 5% aqueous solution of phenol. Chemical oxygen demand was measured at different pH: 4,5,6,7 and varying % of toluene: 20, 30, 40. After extraction with organic solvent, two separate layers were formed; one of toluene + phenol (organic) and the other of water + some amount of phenol (aqueous). Optimum experimental conditions were found at 7 pH and 20% toluene concentration. At these conditions, the highest 60% phenol removal was obtained for 5% aqueous solution of phenol and 68% phenol removal was obtained for actual pharmaceutical wastewater.