Potassium Carbonate → HCID 178515692、化合物
反応式
C([N:4]1[C:8]2=[N:9][C:10]([O:13]C(=O)C)=[CH:11][CH:12]=[C:7]2[CH:6]=[CH:5]1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO.O>[NH:4]1[C:8]2=[N:9][C:10]([OH:13])=[CH:11][CH:12]=[C:7]2[CH:6]=[CH:5]1参加物
4
実験手順
A mixture of acetic acid 1-acetyl-1H-pyrrolo[2,3-b]pyridin-6-yl ester (4.0 g, 18.3 mmol) and potassium carbonate (10.45 g, 75.7 mmol) in methanol/water (50%, 260 mL) was stirred at room temperature for 12 h. The reaction mixture was concentrated to half its volume and extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate and evaporated. The residue was purified by flash column chromatography (silica gel from QingDao, 200-300 mesh, 10% methanol/dichloromethane) afforded 1H-pyrrolo[2,3-b]pyridin-6-ol (1.52 g, 62%): LC/MS m/e calcd for C7H6N2O [M+H]+ 135.14, observed 135.0.
後処理
- concentrationThe reaction mixture was concentrated to half its volume
- extractionextracted with chloroform
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- customevaporated
- customThe residue was purified by flash column chromatography (silica gel from QingDao, 200-300 mesh, 10% methanol/dichloromethane)
出典と根拠
- ORDレコード
- ord-62dbae19759e45a593c7cdaad8ad42d7
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08222416B2
反応ノート
読み込み中…