The reaction of m-chloroperbenzoic (m-CPBA) acid with meso-tetrakis (pentafluorophenyl) porphynatoiron(III) chloride (F20TPPFe(III)Cl ) has been studied in dichloromethane and acetonitrile medium at 25 ± 1°C. The reactive intermediates formed in this reaction have been quantitatively trapped by 2,4,6-tri t-butylphenol (TTBP) in both the solvents. It has been observed that the kinetic plots of the formation of TTBP• radical in dichloromethane are all multiexponential, supporting the formation of more than one reactive intermediate in this solvent. In acetonitrile solvent the formation of TTBP• radical was however observed to be distinctly single exponential. Different kinds of reactive intermediates are proposed in these two solvents.