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Described herein is a photoactivation decaging method of isobutylene\u2010caged thiols through a UV\u2010initiated thiol\u2010ene reaction. The method was demonstrated with an isobutylene\u2010caged cysteine, cyclic disulfide\u2010peptide, and thiol\u2010containing drug, all of which were rapidly and efficiently released under mild UV irradiation in the presence of thiol sources and a photoinitiator. 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