Allyl bromide → 1-Allylpiperazine

HRID 8933

반응식

HRID 8933 반응식
F[C:2](F)(F)[C:3]([N:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)=O.[CH2:13](Br)C=C.C(=O)([O-])[O-].[K+].[K+]>CC#N>[CH2:3]([N:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)[CH:2]=[CH2:13]

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 7172020Trifluoroacetylpiperazine

생성물 1

HCID 8064221-Allylpiperazine수율 155.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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.

후처리

  1. concentrationThe reaction was concentrated under reduced pressure
  2. additiondiluted with CH2Cl2 (30 mL) and water (30 mL)
  3. extractionthe aqueous layer extracted with CH2Cl2 (2×20 mL)
  4. dry with materialThe combined organic extracts were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-32ee4c940d754b23bf862be162c61ba9
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091217B2

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