Reaktion #1605383

ord-ae075176df5c4913b973d43369b5e731

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat 0° C
  2. 2
    EinengenAfter concentration in vacuo the residue
  3. 3
    Sonstigewas partitioned between dichloromethane and saturated aqueous NaHCO3
  4. 4
    WaschenThe organic layer was washed with water
  5. 5
    Trocknendried over MgSO4
  6. 6
    Filtrationfiltered
  7. 7
    Sonstigethe solvent evaporated under reduced pressure

Vorschrift

To a solution of [2-(4-amino-phenyl)-ethyl]-carbamicacid tert-butyl ester (10.75 g, 45.49 mmol) in pyridine (125 ml) at 0° C. 4-Isopropyl-benzenesulfonyl chloride (10.45 g, 47.76 mmol) was added. The mixture was stirred at 0° C. for 1 h and 16 h at room temperature. After concentration in vacuo the residue was partitioned between dichloromethane and saturated aqueous NaHCO3. The organic layer was washed with water, dried over MgSO4, filtered and the solvent evaporated under reduced pressure to give the product as a brown oil (20.82 g, 50%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08232426B2uspto-grants-2012_07