Summary: Peroxide‐containing chitosan was synthesized using a polymer‐analogous reaction between chitosan and tert‐butylperoxymethyl ester of maleic acid. Peroxide‐containing chitosan macromolecules cross‐link into a polymeric hydrogel network in the presence of 1‐vinyl‐2‐pyrrolidone upon heating. Polymeric hydrogels are formed due to reactions of radical chain transfer and recombination. Reacting radical species are chitosan macroradicals and poly(vinylpyrrolidone) macroradicals formed by decomposition of peroxide‐containing fragments. Synthesized hydrogels are pH‐responsive and facilitate drug release.

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