(±)-O-methylperezone (1b) was obtained by selective oxidative demethylation of (±)- leucoperezone trimethyl ether (4a). Compound (4a) was prepared by condensation of 2, 3, 5- trimethoxytoluene (5e) with 6-methyl-5-hepten-2-one, followed by reductive removal of the tertiary alcohol. The aromatic precursor 5e was prepared in four steps from 2, 3- dimethoxytoluene (5a) and, alternatively, in three steps from 5-bromoveratraldehyde (6a). ...