We have prepared a Pd-MgO sample by self-sustaining reaction between Mg and NO, and two Pd-Mg bicomponent alloys by mechanochemical synthesis induced by ball milling. They were characterized by XRD, DSC and XPS techniques. Further characterization was carried out following controlled oxidation which was necessary to enhance the catalytic performance in the; synthesis of methyl isobutyl ketone, Complex transformations characterized in most cases by he formation of Pd-Mg intermetallics are observed by XRD. A common feature of all samples is the surprisingly low concentration of the metallic components due to oxygen and carbon impurities and the lack of palladium on the surface, High catalytic activities were achieved in catalytic studies but overhydrogenation due to the high hydrogenating ability of Pd resulted in decreased selectivities.