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The first facile and efficient Zn(OTf) 2 -catalyzed direct coupling of unprotected propargylic alcohols with arylphosphine oxides has been developed, affording a general, one-step approach to access structurally diverse γ-ketophosphine oxides via sequential Meyer-Schuster rearrangement/phospha-Michael reaction along with new C(sp 3 )-P and C═O bond formations, operational simplicity, and complete atom economy under ligand-free and base-free conditions.