Reaktion #9029

ord-32ee4c940d754b23bf862be162c61ba9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction was concentrated under reduced pressure
  2. 2
    workup.ADDITIONdiluted with CH2Cl2 (30 mL) and water (30 mL)
  3. 3
    Extraktionthe aqueous layer extracted with CH2Cl2 (2×20 mL)
  4. 4
    TrocknenThe combined organic extracts were dried (Na2SO4)
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated in vacuo

Vorschrift

To a stirred solution of 2,2,2-trifluoro-1-piperazin-1-yl-ethanone (515 mg, 2.83 mmol) in dry CH3CN (6 mL) was added allyl bromide (0.32 mL, 3.7 mmol) and powdered potassium carbonate (0.78 g, 5.65 mmol) and the mixture stirred overnight. The reaction was concentrated under reduced pressure, diluted with CH2Cl2 (30 mL) and water (30 mL) and the aqueous layer extracted with CH2Cl2 (2×20 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated in vacuo to afford the crude di-protected piperazine (0.554 g) which was used without further purification in the next reaction.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091217B2uspto-grants-2006_08