Vinyl triflates have been converted into γ'-hydroxy-α, β-enones through their palladium- catalysed coupling with 1-butyn-4-ols followed by the reaction of the obtained 1-hydroxy-3- yn-5-enes in an acidic CH2Cl2/3 N HCl two-phase system in the presence of the n- BuN4Cl/PdCl2 combination. Both the coupling step and the conversion of the carbon-carbon triple bond into the ketonic group have been performed at room temperature. The ...