Regioselective radiofluorodemercuration of the 6-mercurio derivative 5 with [18F]acetylhypofluorite afforded, after acidic hydrolysis, 6-[18F]fluoro-L-3,4-dihydroxyphenylalanine (6-FD, 1) with a radiochemical yield of 11% (decay corrected and based on the total amount of [18F]F2 recovered from the target). 6-FD was obtained with a chemical and radiochemical purity of greater than 99% and with a level of mercury in the final preparation of less than 20 ppb. Utilization of a remote, semiautomated production system, resulted in the preparation of a sterile, pyrogen-free product suitable for human injection after a synthesis time of 50 min.