Reaction of hydrazine with 2, 5-bis (perfluoroalkyl)-1, 3, 4-oxadiazoles (I) in the absence of a solvent was vigorous, exothermic, and resulted in a wide variety of products not easily separated. Moderation of the reaction was obtained by using alcohol as a solvent and lowering the reaction temperature to 0". Under these conditions, good yields of N2-(cr- hydrazonoperfluoroalky1) perfluoroacylhydrazides (11) were isolated (Scheme I).