Mono-or diacetylation of some methoxyhydroxybenzenes and their esters was found dependent on (1) the presence or absence of acetic anhydride in the solvent acetic acid and (2) the availability of two unsubstituted positions ortho to a free hydroxyl or ester group. 2, 4- Dinitrophenyl ethers, like methyl ethers, monoacetylate with selective cleavage of the methoxyl ortho to the acetyl group.