Reaktion #607440
ord-15b6b7f4129b4f74952914e02c45668f
Reaktionsgleichung
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1Sonstigequenched carefully by the addition of a saturated aqueous ammonium chloride solution (150 mL)
- 2ExtraktionThe extraction
- 3WaschenThe combined organic layers were washed with brine (200 mL)
- 4Trocknendried over anhydrous Na2SO4
- 5Filtrationfiltered
- 6SonstigeThe solvent was removed in vacuo
Vorschrift
To a colorless stirred solution of 3′,5′-difluoroacetophenone (50.00 g, 320.24 mmol) in methanol (320 mL), sodium borohydride (3.41 g, 86.47 mmol, 0.27 eq) was added portion wise over 20 minutes at room temperature under inert atmosphere (Ar). Then the reaction mixture was stirred for 45 min at room temperature and then quenched carefully by the addition of a saturated aqueous ammonium chloride solution (150 mL). The extraction was carried out with ethyl acetate (2×200 mL). The combined organic layers were washed with brine (200 mL), dried over anhydrous Na2SO4 and filtered. The solvent was removed in vacuo to give the title compound (50.29 g, 99%) as a colorless oil. The alcohol was used as such in the subsequent step.