REDUCTION of methoxybenzene derivatives by the sodium–ammonia–alcohol reagent followed by acid hydrolysis leads to the formation of a number of hitherto inaccessible unsaturated ketones1. The process fails with some compounds because of their insolubility in liquid ammonia, a typical example being hexaestrol dimethyl ether (I, R = CH3). This substance has been treated under a variety of conditions and with admixed solvents, for example, ether or ethylenediamine, but so far without success.