A convenient and efficient C(sp3)–H phosphorylation has been achieved via the metal-free DDQ-mediated cross-dehydrogenative coupling between diarylphosphine oxides and xanthene derivatives at room temperature. This transformation provides a direct synthetic route to the construction of C(sp3)–P bonds with good functional group compatibility, leading to the formation of alkylphosphonates in up to 96% yield.
