Methyl morpholine oxide → 4-Bromo-6-chloropyridine-3-carbaldehyde
反応式
[Br:1][C:2]1[C:7]([CH2:8]Br)=[CH:6][N:5]=[C:4]([Cl:10])[CH:3]=1.C[N+]1([O-])CC[O:15]CC1>C(#N)C.CCOC(C)=O>[Br:1][C:2]1[C:7]([CH:8]=[O:15])=[CH:6][N:5]=[C:4]([Cl:10])[CH:3]=1参加物
5
実験手順
A flask was charged with 4-bromo-5-(bromomethyl)-2-chloropyridine (490 mg, 1.72 mmol), powdered 4 Å molecular sieves, and NMO (2.19 g, 18.74 mmol) then diluted with ACN (17 mL) and stirred at room temperature for 1 h. The reaction mixture was diluted with EtOAc, filtered, and concentrated in vacuo. The crude residue was purified by silica gel column chromatography (0-20% EtOAc/Hex gradient) to afford the desired product. LCMS-ESI+: calc'd for C6H4BrClNO 219.9 (M+H+); Found: 220.0 (M+H+).
後処理
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe crude residue was purified by silica gel column chromatography (0-20% EtOAc/Hex gradient)
出典と根拠
- ORDレコード
- ord-1d35b466a0b04c46a5f7a704dd95f759
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08987250B2
反応ノート
読み込み中…