Under two-phase conditions, the extraction/removal of phenol from an aqueous alkaline medium via reaction with allyl bromide dissolved in dichloromethane was investigated in this study using tetra-n-butylammonium bromide as a phase-transfer catalyst. The concentrations of base, reactant and catalyst, and solvents were evaluated to find the optimum condition in this reaction. In examining 10 kinds of phase-transfer catalysts, aliquat 336, tetra-n-butylammonium iodide, tetra-n-butylphosphonium bromide, and benzyltributylammonium bromide were found to be the best for increasing the volumetric rate of extraction. The extractive efficiency of phenol increased with increasing basic concentration and was significantly influenced by the activity of solvent. The conversion of phenol in a batch-agitated reactor was found to be more than 99% under suitable conditions of catalyst, solvent, reactant, and basic concentration.