The synthesis of 3-methylalkane-2, 4-diones, which are intense strawlike and fruit-flavored compounds, has been performed by the aldol condensation of n-alkanal (C2-C7) and methyl ethyl ketone to give 4-hydroxy-3-methyl-2-alkanones in 31-72% yield, followed by oxidation using sodium hypochlorite in the presence of 4-benzoyloxy-2, 2, 6, 6-tetramethyl-piperidine- N-oxide in 60-86% yield.