Trifluoroacetic acid → 4-[(E)-2-(4-hydroxyphenyl)vinyl]-1-{4-[2-(1-pyrrolidinyl)-ethoxy]phenyl}-1H-pyridin-2-one

HRID 15054ノート

反応式

HRID 15054 の反応式
FC(F)(F)C(O)=O.CC([O:12][C:13]1[CH:18]=[CH:17][C:16](/[CH:19]=[CH:20]/[C:21]2[CH:26]=[CH:25][N:24]([C:27]3[CH:32]=[CH:31][C:30]([O:33][CH2:34][CH2:35][N:36]4[CH2:40][CH2:39][CH2:38][CH2:37]4)=[CH:29][CH:28]=3)[C:23](=[O:41])[CH:22]=2)=[CH:15][CH:14]=1)(C)C>>[OH:12][C:13]1[CH:18]=[CH:17][C:16](/[CH:19]=[CH:20]/[C:21]2[CH:26]=[CH:25][N:24]([C:27]3[CH:32]=[CH:31][C:30]([O:33][CH2:34][CH2:35][N:36]4[CH2:37][CH2:38][CH2:39][CH2:40]4)=[CH:29][CH:28]=3)[C:23](=[O:41])[CH:22]=2)=[CH:15][CH:14]=1

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 684300224-((E)-2-{4-[(2-methyl-2-propyl)oxy]phenyl}vinyl)-1-{4-[2-(1-pyrrolidinyl)ethoxy]phenyl}-1H-pyridin-2-one

生成物 1

HCID 684306454-[(E)-2-(4-hydroxyphenyl)vinyl]-1-{4-[2-(1-pyrrolidinyl)-ethoxy]phenyl}-1H-pyridin-2-one収率 92.7%

実験手順

Trifluoroacetic acid (2 mL) was added to 4-((E)-2-{4-[(2-methyl-2-propyl)oxy]phenyl}vinyl)-1-{4-[2-(1-pyrrolidinyl)ethoxy]phenyl}-1H-pyridin-2-one (120 mg, 0.26 mmol) and stirred at room temperature for 30 minutes. After concentrating the reaction liquid under reduced pressure, chloroform was added to the reaction liquid which then was washed with aqueous sodium hydrogencarbonate solution and dried over anhydrous sodium sulfate. Concentrating the solvent under reduced pressure, the title compound (97 mg, 92%) was obtained as a white solid.

後処理

  1. concentrationAfter concentrating
  2. customthe reaction liquid under reduced pressure, chloroform
  3. additionwas added to the reaction liquid which
  4. washthen was washed with aqueous sodium hydrogencarbonate solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationConcentrating the solvent under reduced pressure

出典と根拠

ORDレコード
ord-241179f0589349129fa9c34052951db9
出典データセット
uspto-grants-2010_06
特許番号
US07732456B2

反応ノート

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