Fluorine-18 acetyl hypofluorite, produced by a gas/solid-phase reaction, was reacted with D-glucal in water, followed by treatment with HCl and serial passage through columns of charcoal, ion-retardation resin, and alumina. The product was an injectable solution of 2-[18F]fluoro-2-deoxy-D-glucose. The radiochemical purity was greater than 95% and the radiochemical yield was about 40%. The synthesis was completed in about 15 min. Acetyl hypofluorite was shown to be a stable, highly stereoselective fluorinating agent in aqueous systems over a wide pH range.