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A novel type of supported copper(II) catalyst was prepared by the treatment of a Zn–Al layered double hydroxide containing 2,2′-bipyridine-5,5′-dicarboxylate (BDC) anions with a solution of CuCl₂ in ethanol. The Cu loading in the recovered material, designated as LDH-BDC/Cu, was ca. 4%, with an approximate BDC:Cu:Cl molar ratio of 2:1:1. The catalytic performance of LDH-BDC/Cu was examined in the liquid-phase oxidation of styrene, ethylbenzene, cyclohexane and cyclooctane at room temperature, using acetonitrile/water as solvent, and hydrogen peroxide (30%) or tert-butyl hydroperoxide (70%) as terminal oxidant. The main products were benzaldehyde from styrene (up to 14% yield at 24h), acetophenone from ethylbenzene (up to 8% yield at 24h), and a mixture of cyclohexanol and cyclohexanone from cyclohexane (up to 5% yield at 24h). For styrene oxidation using H₂O₂, benzaldehyde was the …