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Acetic Acid → 4-{[(2S)-2-fluoropropyl]oxy}piperidine

HRID 69126
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HRID 69126 반응식
[F:1][C@@H:2]([CH3:11])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1.C(O)(=O)C>CO.[Pd]>[F:1][C@@H:2]([CH3:11])[CH2:3][O:4][CH:5]1[CH2:6][CH2:7][NH:8][CH2:9][CH2:10]1
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참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 666961134-{[(2S)-2-fluoropropyl]oxy}pyridine

생성물 1

HCID 866943284-{[(2S)-2-fluoropropyl]oxy}piperidine수율 43.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

2.2 g of 4-{[(2S)-2-fluoropropyl]oxy}pyridine was added to a solution of 22 mL of acetic acid in 22 mL of methanol, and 500 mg of 10% palladium on carbon (wet type) was added thereto under an argon atmosphere. The mixture was stirred at room temperature overnight under a hydrogen atmosphere of 3 atm. The reaction mixture was filtered through celite and the filtrate was concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (chloroform/methanol) to obtain 988 mg of 4-{[(2S)-2-fluoropropyl]oxy}piperidine.

후처리

  1. additionwas added
  2. filtrationThe reaction mixture was filtered through celite
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by basic silica gel column chromatography (chloroform/methanol)

출처 및 근거

ORD 기록
ord-5bcb731dbce54b409b27b111188b01a7
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822448B2

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