Abstract Hypervalent iodine (λ 5) reagents in combination with p-toluenesulfonic acid when reacted with ketones under reflux temperature in acetonitrile gave α-tosyloxy ketones in moderate to excellent yields. The reaction was developed further for both ketones and dicarbonyl compounds using Dess-Martin periodinane reagent in combination with p- toluenesulfonic acid and methanesulfonic acid, to give mono-α-tosyloxy and mono-α- ...