تفاعل #9029

ord-32ee4c940d754b23bf862be162c61ba9

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe reaction was concentrated under reduced pressure
  2. 2
    workup.ADDITIONdiluted with CH2Cl2 (30 mL) and water (30 mL)
  3. 3
    استخلاصthe aqueous layer extracted with CH2Cl2 (2×20 mL)
  4. 4
    تجفيفThe combined organic extracts were dried (Na2SO4)
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated in vacuo

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091217B2uspto-grants-2006_08