Reaktion #61478

ord-3680548be0b54ada8f1c647f6c494cc6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was evaporated to dryness in vacuo
  2. 2
    Sonstigepartitioned between ethyl acetate (50 ml) and water (50 ml)
  3. 3
    Extraktionre-extracted with ethyl acetate (2×30 ml)
  4. 4
    TrocknenThe combined basic organic extracts were dried over sodium sulfate
  5. 5
    Sonstigeevaporated in vacuo

Vorschrift

A mixture of 3-(tert-butyloxycarbonyl)-7-cyano-2,3,4,5-tetrahydro-1H-3-benzazepine (765 mg, 2.81 mmol) and trifluoroacetic acid (2 ml), in dichloromethane (20 ml) was stirred at 40° C. for 1 h. The reaction mixture was evaporated to dryness in vacuo and partitioned between ethyl acetate (50 ml) and water (50 ml). The aqueous layer was basified using potassium carbonate and re-extracted with ethyl acetate (2×30 ml). The combined basic organic extracts were dried over sodium sulfate and evaporated in vacuo to give the title compound as a colourless oil (212 mg, 44%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07429579B2uspto-grants-2008_09