A Polyniobotungstate-Based Hybrid for Visible-Light-Induced Phosphorylation of N -Aryl-Tetrahydroisoquinoline.

A new organic-inorganic hybrid based on a Nb/W mixed-addendum polyoxometalate with the formula H 14 [(Co(H 2 O) 3 ) 2 (C 10 H 8 N 2 ) 4 (P 4 W 30 Nb 6 O 123 )]·4(C 10 H 8 N 2 )·8H 2 O ( Co - POM ) has been synthesized by the solvothermal method and characterized by single-crystal X-ray diffraction (XRD), powder X-ray diffraction (PXRD), elemental analysis, FTIR spectroscopy, UV-vis absorption spectrum, and thermogravimetric analysis (TGA). Importantly, visible-light-absorption peaks around 525 nm for Co - POM indicated that this material should have potential in visible-light-induced organic reactions. Herein, we disclosed visible-light-promoted phosphorylation of N -aryl-tetrahydroisoquinoline using Co - POM as an efficient heterogeneous photocatalyst. In this procedure, diverse phosphorus reagents are compatible at room temperature and in an O 2 atmosphere, giving the corresponding products in good to excellent yields (up to 97%). Simultaneously, this heterogeneous photocatalyst can be recycled up to ten times with a negligible decrease in yield, showing outstanding sustainability and recyclability.