In order to synthesize MgAl 2 O 4 , three methods were used: (a) a solid phase reaction of MgO and γ-Al 2 O 3 oxides at 900°C for 24h (ceramic method), (b) wet milling during 24h of the mixture of oxides followed by the reaction at 900°C for 12h (mechanochemical synthesis), and (c) coprecipitation of Mg(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 ·9H 2 O with ammonia solution followed by a calcination in a flow of air at 800°C during 4h (coprecipitation method). The synthesized materials were characterized by XRD, BET isotherm, isopropanol dehydration reaction, TGA/DTA and SEM. The results indicate that in all the cases the MgAl 2 O 4 spinel was formed. Besides, a residue of MgO in the samples obtained by the ceramic method and mechanochemical synthesis was found, which was eliminated by purification. The surface area of MgAl 2 O 4 obtained by mechanochemical synthesis and coprecipitation method are much higher than that of the spinel synthesized by the ceramic method. Pt (0.3%) catalysts were prepared by impregnating the three supports with H 2 PtCl 6 . The metallic dispersion of Pt/MgAl 2 O 4 obtained by mechanochemical synthesis was higher than that of Pt catalysts supported on the other spinels, in agreement with the catalytic behavior observed in n-butane dehydrogenation reaction and test reactions of the metallic phase.