A hybrid complex Zr(PO4)(AgHPO4) was prepared by ion-exchange and its activity was examined on the allylic oxidation of cycloolefins using tert-butylhydroperoxide (TBHP) as oxidant under argon atmosphere. Under these reaction conditions, attack of the activated C-H bond was preferred instead of the epoxidation of C=C bond, yielding enols as the main products, this is a novel highly active/selective and reusable heterogeneous catalyst.