Reaktion #1109861

ord-7a057b0da6af43a19026b3f4308b5e4f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated under reduced pressure
  2. 2
    Extraktionthe residue was extracted with ethyl acetate and water
  3. 3
    WaschenThe organic layer was washed with brine
  4. 4
    Trocknendried over anhydrous sodium sulfate
  5. 5
    SonstigeThe solvent was evaporated under reduced pressure

Vorschrift

To a mixed solution of (6R,7R)-4-(tert-butoxycarbonyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-6-carboxylic acid (0.82 g) in toluene (10 ml) and methanol (2 mL) was added trimethylsilyldiazomethane (1.576 mL, 2 mol/l hexane solution) at 0° C. and the mixture was stirred for 30 min. Acetic acid was added until the solution became colorless. The solvent was evaporated under reduced pressure, and the residue was extracted with ethyl acetate and water. The organic layer was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (0.51 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08722662B2uspto-grants-2014_05