The photochemical decarbonylation and coupling of acyl fluorides containing perfluoroalkyl and perfluoro (oxa) alkyl chains have been re-examined. The reaction on either single acyl fluorides or on their binary mixtures has allowed the formation and isolation of macromolecular perfluoro (oxa) alkanes having interesting physical–chemical properties. These perfluoropolyethers are also useful as model compounds and standards to better ...