Abstract The reaction of perfluoroalkylmethanols (RF CH 2 OH) with tris (dimethylamino) phosphine in the presence of excess carbon tetrachloride produces the corresponding perfluoroalkylmethyleneoxy (trisdimethylamino) phos-phonium chlorides in good yield. Exchange of anion chloride is effected, in aqueous solution, by nucleophilic or non- nucleophilic anions (N 3−, SCN−, NCO−, PF 6−) via selective extraction or precipitation. ...