Magnetically retrievable CuFe2O4 and Fe3O4 nanoparticles as efficient catalysts for selective syn diacetoxylation of alkenes have been achieved using PhI(OAc)2 as oxidant under mild conditions. In addition, by using this protocol, different kinds of terminal alkynes were efficiently converted into the corresponding α‐acetoxy ketones. The catalysts were reused with consistent activity up to five cycles. To the best of our knowledge, CuFe2O4 and Fe3O4 heterogeneous catalyzed diacetoxylation of alkenes has not been studied so far.
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