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

HRID 1837723
ノート
印刷プレビュー

反応式

HRID 1837723 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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
  • 出典と根拠

    ORDレコード
    ord-b1437d05714c4e428c6059b7aab18ff2
    出典データセット
    uspto-grants-2004_08
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US06784192B2

    反応ノート

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