Hydrogen Peroxide → 2-Bromo-6-methylpyridine 1-oxide
反応式
[OH:1]O.[Br:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[N:5]=1>C(O)(=O)C>[Br:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[N+:5]=1[O-:1]参加物
4
反応条件
- 温度
- 90 °C
実験手順
Hydrogen peroxide (30%, 1.76 mL, 17.4 mmol) was added to a solution of 2-bromo-6-methyl-pyridine (1.0 g, 5.80 mmol) in acetic acid (20 mL), and heated for 24 h at 90° C. The reaction mixture was cooled to ambient temperature, and partitioned between dichloromethane and water. The aqueous phase was separated and extracted with dichloromethane. The combined organic phases were washed thoroughly with water and dried over anhydrous sodium sulfate. Concentration in vacuo afforded 2-bromo-6-methyl-pyridine 1-oxide (820 mg, 75%) as a brown liquid which was used in the next step without further purification.
後処理
- temperatureThe reaction mixture was cooled to ambient temperature
- custompartitioned between dichloromethane and water
- customThe aqueous phase was separated
- extractionextracted with dichloromethane
- washThe combined organic phases were washed thoroughly with water
- dry with materialdried over anhydrous sodium sulfate
- concentrationConcentration in vacuo
出典と根拠
- ORDレコード
- ord-e7ec2c1329ad4d029fdc28cbdb7d8051
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524705B2
反応ノート
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