Abstract Diazotization of 5-(acetoxyethyl)-2-amino-4-methylselenazole with nitrosoborofluoride in the presence of sodium fluoride in fluoboric acid solution furnishes 5- (acetoxyethyl)-2-fluoro-4-methylselenazole and the corresponding 2-hydroxy compound. Despite low yields, this was the first time that a Sandmeyer-Schiemann reaction has been carried out successfully with 2-aminoselenazoles.