Hydrochloric Acid → HCID 178524942、化合物
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:10]([C:11]([O:13]C)=[O:12])=[N:9][NH:8][C:5]2=[N:6][CH:7]=1.Cl>[OH-].[Na+]>[Br:1][C:2]1[CH:3]=[C:4]2[C:10]([C:11]([OH:13])=[O:12])=[N:9][NH:8][C:5]2=[N:6][CH:7]=1参加物
4
反応条件
- 温度
- 90 °C
実験手順
A suspension of methyl 5-bromo-1H-pyrazolo[3,4-b]pyridine-3-carboxylate (VII) (70 mg, 0.27 mmol) in aqueous 1N NaOH solution (20 mL) was heated at 90° C. for 3 h until the solution became clear. The solution was then cooled to 0° C. and acidified with a 10% HCl solution. The solids formed were filtered, washed with cold water and dried at room temperature under vacuum to give 5-bromo-1H-pyrazolo[3,4-b]pyridine-3-carboxylic acid (VIII) as a white solid (60 mg, 0.25 mmol, 92% yield). 1H NMR (CDCl3) δ ppm 8.58 (d, J=3.01 Hz, 1H), 8.66 (d, J=3.01 Hz, 1H); ESIMS found for C7H4BrN3O2 m/z 242.1 (M+H).
後処理
- temperatureThe solution was then cooled to 0° C.
- customThe solids formed
- filtrationwere filtered
- washwashed with cold water
- customdried at room temperature under vacuum
出典と根拠
- ORDレコード
- ord-1c4a5887cf984d6c9080d88f676d5525
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09446035B2
反応ノート
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