Sodium methanethiolate → 6-Methylsulfanyl-[2,3']bipyridin-3-ol
反応式
F[C:2]1[N:7]=[C:6]([C:8]2[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=2)[C:5]([O:14]C)=[CH:4][CH:3]=1.[CH3:16][S-:17].[Na+]>CN(C)C=O>[CH3:16][S:17][C:2]1[N:7]=[C:6]([C:8]2[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=2)[C:5]([OH:14])=[CH:4][CH:3]=1参加物
4
反応条件
- 温度
- 160 °C
実験手順
6-Fluoro-3-methoxy-[2,3′]bipyridine (30 mg) and sodium thiomethoxide (103 mg) were suspended in N,N-dimethylformamide (1.5 ml), and the suspension was stirred at 160° C. for 4 hr. The reaction solution was cooled to room temperature, the reaction solution was filtered, and the solvent was removed from the filtrate by distillation under the reduced pressure. The residue was purified by thin layer chromatography using chloroform-methanol to give 6-methylsulfanyl-[2,3′]bipyridin-3-ol (13 mg, yield 45%).
後処理
- temperatureThe reaction solution was cooled to room temperature
- filtrationthe reaction solution was filtered
- customthe solvent was removed from the filtrate by distillation under the reduced pressure
- customThe residue was purified by thin layer chromatography
出典と根拠
- ORDレコード
- ord-2ef3d7694a8d4bcab706b166e0ceb66a
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07560558B2
反応ノート
読み込み中…