반응 #9029

ord-32ee4c940d754b23bf862be162c61ba9

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction was concentrated under reduced pressure
  2. 2
    workup.ADDITIONdiluted with CH2Cl2 (30 mL) and water (30 mL)
  3. 3
    추출the aqueous layer extracted with CH2Cl2 (2×20 mL)
  4. 4
    건조The combined organic extracts were dried (Na2SO4)
  5. 5
    여과filtered
  6. 6
    농축concentrated in vacuo

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091217B2uspto-grants-2006_08