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A photo-labile compound that is bioinactive but upon irradiation with light yields bioactive species, is called as “caged compound” (
1
) (
see
Scheme 1). Photolysis of caged compounds generating bioactive species, i.e., “uncaging,” has become a general method to produce a desired amount of bioactive species in a specific time interval at desired place or area of the target biological systems (
1
,
2
). This chapter deals with two caged free radicals: a caged hydroxyl radical, i.e., photo-Fenton reagent, and caged nitric oxides (NOs). Uncaging of these caged free radicals yield hydroxyl radical and NO, respectively, which are believed to be associated with free-radical tissue damage.