In this work, the synthesis of gallic acid-chitosan and catechin-chitosan conjugates was carried out by adopting a free radical-induced grafting procedure. For this purpose, an ascorbic acid/hydrogen peroxide redox pair was employed as radical initiator. The formation of covalent bonds between antioxidant and biopolymer was verified by performing UV, FT-IR, and DSC analyses, whereas the antioxidant properties of chitosan conjugates were compared with that of a blank chitosan, treated in the same conditions but in the absence of antioxidant molecules. The good antioxidant activity shown by functionalized materials proved the efficiency of the reaction method.