Hypervalent Iodine(III)‐Mediated Oxidative Decarboxylation of β‐Keto Acids

Abstract Oxidative decarboxylation of β‐keto acids mediated by hypervalent iodine(III) reagents is described. This decarboxylative C−O bond‐forming reaction uses a combination of (diacetoxyiodo)benzene and an aliphatic carboxylic acid to give the corresponding α‐acyloxy ketones. Preliminary mechanistic studies suggest that the reaction proceeds through a ligand coupling followed by decarboxylation. This reaction offers an attractive alternative to existing methods for the exclusive synthesis of α‐acyloxy ketones.