Hydrochloric Acid → 2-(1H-pyrazolo(3,4-b)pyridin-1-yl)acetic acid
反応式
C([O:3][C:4](=[O:15])[CH2:5][N:6]1[C:10]2=[N:11][CH:12]=[CH:13][CH:14]=[C:9]2[CH:8]=[N:7]1)C.O[Li].O.Cl>C1COCC1.O>[N:6]1([CH2:5][C:4]([OH:15])=[O:3])[C:10]2=[N:11][CH:12]=[CH:13][CH:14]=[C:9]2[CH:8]=[N:7]1参加物
6
実験手順
To a stirred solution of pyrazolo[3,4-b]pyridin-1-yl-acetic acid ethyl ester (210 mg, 1.02 mmol) (Preparation 133) in THF (4 mL) and water (1 mL) at 0° C. was added LiOH.H2O (129 mg, 3.06 mmol). The reaction mixture was stirred at room temperature for 2 hours. The pH was of the mixture was adjusted to pH 4 with 2 N aqueous hydrochoric acid and extracted with 20% isopropanol in dichloromethane (8×5 mL). The combined organics were dried over sodium sulfate, filtered and concentrated under reduced pressure to afford the title compound as an off-white solid in 40% yield, 70 mg.
後処理
- extractionextracted with 20% isopropanol in dichloromethane (8×5 mL)
- dry with materialThe combined organics were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0e66acda19e54af7a992eb97e2d0e342
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846698B2
反応ノート
読み込み中…