Fluoroperoxysulfuryl fluoride, FS0200F, was the first compound reported to contain the fluoroperoxy, OOF, group. This compound was prepared1 by the photolytic reaction of sulfur trioxide, S03, and oxygen difluoride, OF2, and by the reaction of sulfur dioxide, S02, and dioxygen difluoride.2 Thompson3 reported that the direct fluorination of salts of trifluoroacetic acid, CFsC02H, produced a number of products including very small amount of fluoroperoxytrifluoromethane, CF3OOF, and fluoroperoxypentafluoroethane, CFS-CF2OOF. 1-and 2-fluoroperoxyperfluoropropanes have also been reported4 5to result from the reaction of perfluoropropene, CsFe, and 02F2. At the time this research was initiated a convenient method for the preparation of a fluoroperoxyperfluoroalkane was not available.Anderson and Fox6 reported that oxygen difluoride, OF2, and carbonyl fluoride, COF2, react in the presence of cesium fluoride, CsF, catalyst to give good yields of bis(trifluoromethyl) trioxide, CF3OOOCF3, and have suggested that the formation of CF3OOOCF3 proceeds by the mechanism COF2 + CsF -> Cs+OCF3-They, however, did not detect CF3OOF in their experiments.We have additional proof of the validity of this mech-