Hydrogen Peroxide → 2-(Trifluoromethyl)pyridine 1-oxide
反応式
[F:1][C:2]([F:10])([F:9])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[OH:11]O>C(O)(=O)C>[F:1][C:2]([F:10])([F:9])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N+:4]=1[O-:11]参加物
4
反応条件
- 温度
- 70 °C
実験手順
To a stirred solution of 2-trifluoromethyl pyridine (5 g, 34 mmol) in acetic acid (25 mL) is added 33% of aqueous H2O2 (20 mL) at room temperature. The reaction mixture is allowed to stir for 12 h at 70° C. After complete consumption of starting material the reaction mixture is concentrated under reduced pressure. The residue is dissolved in chloroform (250 mL) and pH is adjusted to 7 with K2CO3 (20 g approx). Resulting solid is filtered through glass sintered funnel and washed with chloroform. Filtrate is concentrated under reduced pressure to give 2-trifluoromethyl-pyridine 1-oxide as syrupy liquid (4.3 g).
後処理
- customAfter complete consumption of starting material the reaction mixture
- concentrationis concentrated under reduced pressure
- dissolutionThe residue is dissolved in chloroform (250 mL)
- customResulting solid
- filtrationis filtered through glass sintered funnel
- washwashed with chloroform
- concentrationFiltrate is concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-595de53777d74446aa43ab85662dfa98
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08362249B2
反応ノート
読み込み中…