A series of layered double hydroxides (LDHs) materials containing different divalent and trivalent cations [Mg 1−x−y Me x Al y (OH) 2 ] (CO 3 ) y/2 ·mH 2 O, where Me: Cu, Fe, Ni, Zn; were prepared by coprecipitation. The solids were characterized by X-ray diffraction, temperature-programmed reduction (TPR) and temperature-programmed desorption (TPD) of CO 2 ; thermogravimetric and textural analysis were also performed. All solids, dried at 100°C, showed XRD patterns typical of hydrotalcite, where Me cations isomorphically replaced some Mg 2+ cations within the layers, thus forming a ternary LDH, as the starting material. The materials were calcined at 550°C and tested as catalysts in the gas-phase conversion of 4-methylpentan-2-ol at 200°C.