Abstract: Methyl hypofluorite, MeOF, easily made from MeOH and Fz, proved to be an excellent source for the novel electrophilic methoxylium ion 'MeO'”. MeOF was reacted with the enol forms of carbonyls, producing in good to excellent yields the corresponding a- methoxy carbonyl derivatives. It was found that the methoxylation is best carried out on methyl enol ethers. Silyl enol ethers and enol acetates were also tested but with limited ...