Reaktion #426160

ord-32eccf095e224179a96387874a40e7cf

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture heated
  2. 2
    Temperaturat reflux for 30 minutes
  3. 3
    Filtrationfiltered through a pad of Celite
  4. 4
    Waschenwashed with ethanol (30 mL)
  5. 5
    Einengenconcentrated under reduced pressure

Vorschrift

A solution of ethyl benzyl-3-(tert-butoxycarbonylamino)-3-(fluoromethyl)pyrrolidine-1-carboxylate (2.27 g, 6.44 mmol) and ammonium formate (3.03 g, 32.2 mmol) in ethanol (60 mL) was flushed with nitrogen for 15 minutes. 10% Pd/C (0.69 g, 0.644 mmol) was added and the mixture heated at reflux for 30 minutes. The reaction mixture was cooled to ambient temperature, filtered through a pad of Celite and washed with ethanol (30 mL) and concentrated under reduced pressure to afford tert-butyl 3-(fluoromethyl)pyrrolidin-3-ylcarbamate (1.4 g, 100%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08889704B2uspto-grants-2014_11