The first perfluorinated carbohydrate (sugar) has been recently synthesized by carefully controlled reactions of elemental fluorine with the carbohydrate 1,2:3,5-di-O-isopropylidene-D-xylofuranose. We have synthesized the compound perfluoro-1,2:3,5-di-O-isopropylidene-D-xylofuranose. The compound is unambiguously characterized by (19)F NMR and two-dimensional (19)F NMR.