Abstract: 2-Alkylated 1, 4-diketones and a-alkylated g-keto esters can be easily prepared by a two-step procedure which involves first the conjugate addition of a nitroalkane to an enedione derivative in acetonitrile with DBU as base, followed by chemoselective hydrogenation of the C–C double bond (H2, 10% Pd/C) of the Michael adduct, obtained after elimination of nitrous acid. Key words: 2-Alkyl 1, 4-diketones, a-alkyl g-keto esters, ...