Reaktion #90346

Reaktionsgleichung

sodium bicarbonate

sodium borohydride

4-(1-(4-(perfluoroethoxy)phenyl)-1H-1,2,4-triazol-3-yl)benzaldehyde

hydrogen chloride

→

title compound

Ausbeute 100.0%

(4-(1-(4-(perfluoroethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)methanol

Ausbeute 100.0%

Lösungsmittel

ethyl acetate

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic phase separated
2. 2
   Waschenrinsed with saturated aqueous sodium bicarbonate, brine
3. 3
   Trocknendried over magnesium sulfate
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated

Vorschrift

To 4-(1-(4-(perfluoroethoxy)phenyl)-1H-1,2,4-triazol-3-yl)benzaldehyde (WO 2011/017513) (3.00 g, 7.83 mmol) in methanol (40 mL) cooled to 0° C. was added sodium borohydride (0.296 g, 7.83 mmol). The reaction mixture was stirred for 1 hour. The mixture was acidified with aqueous hydrogen chloride (1 N) and diluted with ethyl acetate. The pH was adjusted to 7 by aqueous sodium bicarbonate. The organic phase separated, rinsed with saturated aqueous sodium bicarbonate, brine, dried over magnesium sulfate, filtered, and concentrated to provide the title compound as a solid (3.01 g, 100%): ESIMS m/z 386 ([M+H]+).

Quelle