Hydrogen Peroxide → 2-Bromo-6-methylpyridine 1-oxide
反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[N:3]=1.[OH:9]O>C(O)(=O)C.O>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[N+:3]=1[O-:9]参加物
5
反応条件
- 温度
- 90 °C
実験手順
2-Bromo-6-methylpyridine (36 g, 0.2 mol) was dissolved in acetic acid (700 ml), hydrogen peroxide (30%, 62 ml, 0.6 mol) was added and the mixture was stirred at 90° C. for 24 hours. After cooling to room temperature, the mixture was diluted with water (700 ml) and extracted with DCM (4×). The combined organic phases were washed with water, dried (sodium sulfate) and concentrated under reduced pressure to give 36 g of a red-brown liquid (0.19 mol, 94%) MS(APCI) m/z=188.0 [M+1]+.
後処理
- temperatureAfter cooling to room temperature
- extractionextracted with DCM (4×)
- washThe combined organic phases were washed with water
- dry with materialdried (sodium sulfate)
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0174e97f34374a7eb9ad52ca8502bfa9
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09321724B2
反応ノート
読み込み中…