Reaktion #329012

ord-73cdd00e5afc4df8bb19372bffddee08

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction was filtered
  2. 2
    Waschenthe salts washed with a small amount of acetone
  3. 3
    Sonstigeevaporated gently to concentration
  4. 4
    Waschenwashed with water
  5. 5
    ExtraktionThe aqueous phase was re-extracted with EtOAc
  6. 6
    WaschenThe combined organic layers were washed with brine
  7. 7
    Trocknendried over MgSO4
  8. 8
    FiltrationThe product was filtered
  9. 9
    Sonstigeevaporated to dryness
  10. 10
    Sonstigeto leave a pale orange oil

Vorschrift

To the 1-ethylpiperazine (2.33 g, 20.2 mmol) and K2CO3 (2.79 g, 20.2 mmol) in acetone (27 ml) was added propargyl bromide (2.00 g, 13.5 mmol) dropwise at 0° C. under N2. The reaction was stirred at room temperature overnight. The reaction was filtered and the salts washed with a small amount of acetone. The filtrates were combined and evaporated gently to concentration. The residue was taken up in EtOAc and washed with water. The aqueous phase was re-extracted with EtOAc. The combined organic layers were washed with brine and dried over MgSO4. The product was filtered and evaporated to dryness to leave a pale orange oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08653084B2uspto-grants-2014_02