Reaktion #541710

ord-413d9799cc8d42568db2a8ec6b8f54ea

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    SonstigeThe insoluble substance was removed by filtration
  3. 3
    Sonstigethe solvent was evaporated under reduced pressure
  4. 4
    SonstigeThe obtained residue was purified by silica gel column chromatography [eluent: 95-85% hexane/ethyl acetate]

Vorschrift

To a solution mixture of tert-butyl 4-(2-((tert-butoxycarbonyl)(methyl)amino)phenyl)-2-nitrobenzoate (57 mg) in ethyl acetate (2.5 mL) and methanol (2.5 mL), 10% palladium-carbon (11 mg) was added. The resulting mixture was stirred at room temperature for 3 hours under a hydrogen atmosphere. The insoluble substance was removed by filtration, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: 95-85% hexane/ethyl acetate] to obtain 48 mg of tert-butyl 2-amino-4-(2-((tert-butoxycarbonyl)(methyl)amino)phenyl)benzoate as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08492582B2uspto-grants-2013_07