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

HRID 2376735ノート

反応式

HRID 2376735 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-1b6be7a2289d46d48373e4e885290bf8
出典データセット
uspto-grants-2008_12
特許番号
US07468376B2

反応ノート

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