(5-Bromo-6-methoxypyridin-2-yl)methanol → 5-Bromo-6-methoxypicolinaldehyde
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:10][OH:11])=[N:6][C:7]=1[O:8][CH3:9]>C(Cl)Cl.O=[Mn]=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH:10]=[O:11])=[N:6][C:7]=1[O:8][CH3:9]参加物
4
実験手順
(5-Bromo-6-methoxypyridin-2-yl)methanol of preparation 77 (92 mg, 0.42 mmol) was dissolved in DCM (5 ml). MnO2 (477 mg, 5.49 mmol) was added. The reaction was stirred under nitrogen at room temperature for overnight. LCMS showed ˜30% of the starting material remained, and the reaction continued for another 5 hr at which time ˜15% of the starting material remained by LCMS. The reaction mixture was filtered and the filtrate was evaporated to dryness in vacuo. A brownish solid was obtained (69 mg) which was used in the next step without further purification.
後処理
- filtrationThe reaction mixture was filtered
- customthe filtrate was evaporated to dryness in vacuo
- customA brownish solid was obtained (69 mg) which
- customwas used in the next step without further purification
出典と根拠
- ORDレコード
- ord-f35aa6dabba04ec7bb6621d9f777024c
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08916593B2
反応ノート
読み込み中…