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Hydrochloride methanol → (E)-4-[2-(2-fluorophenyl)vinyl]piperidine

HRID 1837723
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반응식

HRID 1837723 반응식
C(OC([N:6]1[CH2:11][CH2:10][CH:9](/[CH:12]=[CH:13]/[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[F:20])[CH2:8][CH2:7]1)=O)=C.Cl.CO>>[F:20][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1/[CH:13]=[CH:12]/[CH:9]1[CH2:8][CH2:7][NH:6][CH2:11][CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 21893726Hydrochloride methanolHCID 226787831-(vinyloxycarbonyl)-4-[(E)-2-(2-fluorophenyl)-1-ethenyl]piperidine

생성물 1

HCID 22248269(E)-4-[2-(2-fluorophenyl)vinyl]piperidine수율 97.9%

실험 절차

904 mg of 1-(vinyloxycarbonyl)-4-[(E)-2-(2-fluorophenyl)-1-ethenyl]piperidine was suspended in 5 ml of a 10% hydrogen chloride-methanol solution. After stirring for 15 minutes at room temperature, the mixture was heated at 70° C. for one hour. The solvent was evaporated, and water and ethyl acetate were added to the residue, to separate the aqueous layer. The aqueous layer was basified with a diluted ammonia, and extracted with ethyl acetate. The organic layer was washed with water and brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, to give 660 mg of the title compound as a colorless oil.

후처리

  1. temperature
the mixture was heated at 70° C. for one hour
  • customThe solvent was evaporated
  • additionwater and ethyl acetate were added to the residue
  • customto separate the aqueous layer
  • extractionextracted with ethyl acetate
  • washThe organic layer was washed with water and brine
  • dry with materialdried over anhydrous magnesium sulfate
  • customThe solvent was evaporated
  • 출처 및 근거

    ORD 기록
    ord-b1437d05714c4e428c6059b7aab18ff2
    출처 데이터셋
    uspto-grants-2004_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06784192B2

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