A variety of phenols have been obtained in aqueous media with moderate to excellent chemical yields (≤100%) by using arylboronic acids and esters as substrates, a robust CdS-TiO2 nanohybrid as a heterogeneous photocatalyst, visible light irradiation (467 nm), and an O2-saturated atmosphere. The nanohybrid was prepared through a linker-assisted methodology that uses mercapto alkanoic acids as the organic linkers. The nanohybrid showed improved photocatalytic activity in the hydroxylation of substituted arylboronic acids and phenyl boronic esters compared with that of pristine CdS quantum dots. The nanohybrid can be reused in up to five photocatalytic cycles with ∼90% of its outstanding activity preserved.