Cerium (IV)-mediated intermolecular direct biaryl coupling of aromatic tertiary amines and naphthol via dual C-H bond activation has been reported. The new C-C bond is formed regioselectively ortho to the amino and hydroxyl substituents under oxidative conditions to give substituted bifunctional amino naphthols. We report here the use of Ce-MCM-41 catalyst for the synthesis of these unsymmetrical biaryls via oxidative cross coupling under mild conditions. The catalyst was recovered by simple filtration and reused for several cycles with consistent activity. (C) 2012 Elsevier B. V. All rights reserved.