PROCESS FOR THE PREPARATION OF LITHIUM PENTAFLUORO(TRIFLUOROMETHYL)PHOSPHATE-DIMETHOXYETHANE(1/2) AND LITHIUM TETRAFLUORO[BIS(TRIFLUOROMETHYL)]PHOSPHATE-DIMETHOXYETHANE(1/2)

摘要

A process for the preparation of lithium pentafluoro(trifluoromethyl)phosphate-dimethoxyethane(1/2) and lithium tetrafluoro[bis(trifluoromethyl)]phosphate-dimethoxyethane(1/2) of general formula Li[(CF)PF]x 2CHOCHCHOCH, wherein n=1, 2, consists in addition of lithium fluoride to tetrafluoro(trifluoromethyl)]phosphoran or tetrafluoro[bis(trifluoromethyl)]phosphoran in the medium of dimethoxyethane at and trifluoromethylation of trivalent phosphorus amidochlorides by means of Ruppert system CFBr/P(NEt). Prepared amides of trifluoromethyl and bis(trifluoromethyl) phosphonous acids under action of gaseous chlorine hydride are converted to corresponding chlorides of trifluoromethyl and bis(trifluoromethyl) phosphonous acids, upon chloration thereof tetrachloro(trifluoromethyl)]phosphoran and tetrachloro[bis(trifluoromethyl)]phosphoran are prepared, and after interaction of those with zinc fluoride tetrafluoro(trifluoromethyl)]phosphoran and tetrafluoro[bis(trifluoromethyl)]phosphoran are prepared. Further reaction with lithium fluoride in dimethoxyethane medium results in the preparation of desired lithium pentafluoro(trifluoromethyl)phosphate-dimethoxyethane(1/2) and lithium tetrafluoro[bis(trifluoromethyl)]phosphate-dimethoxyethane(1/2), which are separated by conventional methods.