反应详情

(S)-3,3,3-Trifluoro-2-hydroxy-2-methylpropionic acid (1.00 g) was dissolved in tetrahydro-furan (10.0 ml), and thereto were added successively benzotriazol-1-yl-oxy-tris-pyrrolidino-phosphonium hexafluorophosphate (3.64 g) and triethylamine (1.80 ml) under ice-cooling, and the mixture was stirred at room temperature. Ten hours later, to the reaction solution was added a 1N aqueous hydrochloric acid solution under ice-cooling, and the mixture was extracted with ethyl acetate. The organic layer was washed successively with a saturated aqueous sodium hydrogen carbonate solution and a saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (the developing solvent: hexane/ethyl acetate=10/1, 5/1) to give the title compound (1.10 g) as a colorless liquid.

1. temperaturecooling
2. temperaturecooling
3. extractionthe mixture was extracted with ethyl acetate
4. washThe organic layer was washed successively with a saturated aqueous sodium hydrogen carbonate solution
5. dry with materiala saturated aqueous sodium chloride solution, dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe obtained residue was purified by silica gel column chromatography (the developing solvent