Abstract 1-Methoxytetrafluoropropionic acid (2) is resolved by diastereomeric amide formation with (S)-(-)-1-phenethylamine/chromatography/hydrolysis. Both enantiomers are obtained in≥ 99% ee. Conversion of each enantiomeric acid to its potassium salt followed by thermolysis in triethylene glycol/1, 3-dimethyl-3, 4, 5, 6-tetrahydro-2 (1H)-pyrimidinone (DMPU) gives the enantiomers of 1, 2, 2, 2-tetrafluoroethyl methyl ether (1) with a very ...