Reaktion #426200

ord-6de5baf49a4e461b89aedd3d90c3117e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux under nitrogen for 3 hours
  3. 3
    TemperaturAfter cooling
  4. 4
    Filtrationthe reaction mixture was filtered through Celite®
  5. 5
    EinengenThe filtrate was concentrated under reduced pressure
  6. 6
    Filtrationfiltered through Celite again
  7. 7
    SonstigeRemoval of the solvent

Vorschrift

A mixture of (R)-tert-butyl 1-benzyl-3-(hydroxymethyl)pyrrolidin-3-ylcarbamate (387 mg, 1.26 mmol), 10% Pd/C (134 mg, 0.126 mmol), ammonium formate (398 mg, 6.32 mmol) and MeOH (10 mL) was heated at reflux under nitrogen for 3 hours. After cooling, the reaction mixture was filtered through Celite®. The filtrate was concentrated under reduced pressure. The residue was taken up in DCM and filtered through Celite again. Removal of the solvent gave (R)-tert-butyl 3-(hydroxymethyl)pyrrolidin-3-ylcarbamate (260 mg, 95%), which was used in the next Step without further purification.

Quelle

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