Abstract: The synthesis of the first perfluorinated tertiary alkyl hypochlorite,(CF,), COCl, is described along with the new polyfluoroalkyl hypochlorites CH3C (CF3) 20Cl,(CF&CHOCl, and CFCHzOCl. All were prepared by reaction of the corresponding alcohols with chlorine monofluoride. The new hypochlorites react readily and nearly quantitatively with carbon monoxide and with sulfur dioxide to produce the corresponding chloroformates and ...