Potassium Hydroxide → 2-[4,6-Bis(4-fluorophenyl)-5-(4-pyridyl)pyrazolo[3,4-b]pyridin-2-yl]acetic acid

HRID 42576ノート

反応式

HRID 42576 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]3[C:10](=[N:27][N:28]([CH2:30][C:31]([O:33]CC)=[O:32])[CH:29]=3)[N:11]=[C:12]([C:20]3[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=3)[C:13]=2[C:14]2[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=2)=[CH:4][CH:3]=1.[OH-].[K+]>CCO.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]3[C:10](=[N:27][N:28]([CH2:30][C:31]([OH:33])=[O:32])[CH:29]=3)[N:11]=[C:12]([C:20]3[CH:21]=[CH:22][C:23]([F:26])=[CH:24][CH:25]=3)[C:13]=2[C:14]2[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=2)=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 67014566HCID 67014566、化合物

生成物 1

HCID 670143832-[4,6-Bis(4-fluorophenyl)-5-(4-pyridyl)pyrazolo[3,4-b]pyridin-2-yl]acetic acid収率 66%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of ethyl 2-[4,6-bis(4-fluorophenyl)-5-(4-pyridyl)pyrazolo[3,4-b]pyridin-2-yl]acetate (0.09 g, 0.2 mmol, obtained in example 32) in EtOH (4.2 mL), a solution of KOH (0.09 g, 2.5 mmol) in water (0.5 mL) was added. This was heated to reflux for 1 h. It was allowed to cool and concentrated. The residue was dissolved in a mixture of EtOAc and water. The phases were separated. The aqueous phase was acidified and extracted with EtOAc. The combined organic phases were dried over Na2SO4 and concentrated to dryness, to afford 57 mg of title compound (yield: 66%).

後処理

  1. temperatureThis was heated
  2. temperatureto reflux for 1 h
  3. temperatureto cool
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in a mixture of EtOAc and water
  6. customThe phases were separated
  7. extractionextracted with EtOAc
  8. dry with materialThe combined organic phases were dried over Na2SO4
  9. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-49040e64fcfd400e89cb671a23c34d54
出典データセット
uspto-grants-2013_09
特許番号
US08536194B2

反応ノート

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