Abstract The useful electrophilic fluorinating agent, acetyl hypofluorite, was obtained by passing F 2 diluted in N 2 through columns containing complexes of alkali metal acetates with acetic acid. Acetyl hypofluorite obtained from KOAc (HOAc) 1.5 and 0.14% F 2 in N 2 was reacted with tri-O-acetyl-D-glucal in CCl 3 F to obtain tetra-O-acetyl-2-deoxy-2-fluoro-D- glucose in 68% yield based on F2. These conditions are appropriate to the radiosynthesis ...