Reaktion #648667

ord-3f7694c970b54369b45e3665c2a5eb88

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe phases were separated
  2. 2
    Waschenthe organic phase was washed with water
  3. 3
    Trocknendried over magnesium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated
  6. 6
    SonstigeThe crude product was purified by flash chromatography on silica gel (mobile phase: toluene/ethyl acetate gradient)

Vorschrift

409 mg (10.8 mmol) of sodium borohydride were added to 2.20 g (9.84 mmol) of the compound from Example 127A in 180 ml of ethanol and 60 ml of ethyl acetate under argon, and the mixture was stirred at 40° C. for 2 h. The reaction mixture was added to dichloromethane, the phases were separated, and the organic phase was washed with water, dried over magnesium sulfate, filtered and concentrated. The crude product was purified by flash chromatography on silica gel (mobile phase: toluene/ethyl acetate gradient) to result in 1.52 g (69% of theory) of a mixture of the diastereomers of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08063234B2uspto-grants-2011_11