Triacetoxyperiodinane → 5-Bromo-2-chloropyridine-3-carbaldehyde
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:9][OH:10])[C:5]([Cl:8])=[N:6][CH:7]=1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[N:6][C:5]([Cl:8])=[C:4]([CH:3]=1)[CH:9]=[O:10]参加物
4
実験手順
To a solution of (5-bromo-2-chloropyridin-3-yl)methanol (6.8 g, 30.6 mmol) in DCM (200 mL), was added Dess-Martin periodinane (32.4 g, 76.6 mmol) at 0° C. The resulting mixture was stirred at room temperature for 12 h. The reaction mixture was concentrated in vacuo and the residue was purified by column chromatography on silica gel (0 to 30% EtOAc in petroleum ether) to afford 5.05 g of 5-bromo-2-chloronicotinaldehyde. LCMS [M+H]+ 221.1.
後処理
- concentrationThe reaction mixture was concentrated in vacuo
- customthe residue was purified by column chromatography on silica gel (0 to 30% EtOAc in petroleum ether)
出典と根拠
- ORDレコード
- ord-732957e950934f0ba4b72d11177a6eb6
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09108944B2
反応ノート
読み込み中…