Abstract A number of N, O-diacylhydroxylamines have been prepared by the reaction of potassium salts of hydroxamic acids with variety of acylating agents which include: benzoyl, p-nitrobenzoyl, anisoyl, p-chlorobenzyl and lauroyl chlorides in dioxane under reflux. The structure of resulting N, O-diacylhydroxylamines has been determined by spectral analysis, Attempted have been made to prepare mixed anhydrides of several N, O- ...