Publisher Summary This chapter discusses the fluorinated hypofluorites and hypochlorites. The richness of the exciting field of fluorinated hypofluorites and hypochlorites is due in very large part to the imaginative work by Ruff and Lustig. Although there are many variations, the three main methods of preparing the alkali-metal fluorides for their catalytic role are thermal dehydration accompanied by mechanical powdering, heating under vacuum, and the formation of a salt, which is subsequently decomposed, for example, the reaction with hexafluoroacetone in acetonitrile. The present chapter is an effort to update the most recent accessible review on fluoroxy compounds and hypofluorites. The use of alkali-metal-fluoride-catalyzed fluorination of appropriate oxygen-containing species enhances the ease of syntheses and the yields of bisfluoroxy compounds.