The activity of the metal–organic framework (MOF) {[CuI(CN)(phen)2·CuII(CN)2·(phen)]·5H2O} containing 1,10-phenanthroline ligand (phen) has been investigated for the oxidation of 3,5-di-tert-butylcatechol (3,5-DTBCH2) to 3,5-di-tert-butyl-o-benzoquinone (3,5-DTBQ) with hydrogen peroxide. The effects of pH and concentration of catalyst, hydrogen peroxide and substrate on the oxidation reaction and yield of the reaction product have been studied. Kinetic studies indicate pseudo first-order rate with respect to the 3,5-DTBCH2 concentration (kobs = 0.113 min−1). Disodium salt of terephthalic acid photoluminescence probing technology indicated the formation of the hydroxyl radical as the reactive oxygen species in the MOF/H2O2—system. A mechanism for the oxidation reaction has been discussed.