Reaktion #92734

ord-6aa1473429484d83946237626c3c6865

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture was filtered over Celite
  2. 2
    Sonstigethe solvent was then evaporated under reduced pressure
  3. 3
    workup.ADDITIONTo the obtained residue were added a saturated aqueous sodium hydrogen carbonate solution and chloroform
  4. 4
    Sonstigea layer separation operation
  5. 5
    Trocknenby drying over anhydrous magnesium sulfate
  6. 6
    SonstigeThe solvent was evaporated under reduced pressure

Vorschrift

To a solution of 280 mg of methyl 3-[(2S)-2-{[(1S)-1-phenylethyl]amino}propyl]benzoate in 6.8 ml of ethanol were added 30 mg of 20% palladium-carbon hydroxide (wet) and 320 mg of ammonium formate, followed by stirring at 80° C. for 4 hours. The reaction mixture was filtered over Celite and the solvent was then evaporated under reduced pressure. To the obtained residue were added a saturated aqueous sodium hydrogen carbonate solution and chloroform to carry out a layer separation operation, followed by drying over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to obtain 180 mg of methyl 3-[(2S)-2-aminopropyl]benzoate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447090B2uspto-grants-2016_09