The one step, simple and rapid oxidation procedure by metachlorperbenzoic acid on certain ring substituted secondary anilines was employed to prepare nitrone functional groups required as potential metabolites and/or intermediates for drug metabolism studies. The structures and purity of purity of nitrones were confirmed using scpectrosopic methods and their separations from both starting products and corresponding primary anilines were achieved by use of thin-layer and high performance liquid chromatographic techniques. Keywords :