Hydrochloric Acid → HCID 11770760, Verbindung

(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

ORD-Eintrag

ord-c787be264e9c4cdd89ba41303c495c5c

Quelldatensatz

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08389511B2