Peracetic Acid → 2-Bromo-6-ethyl-pyridine 1-oxide
反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][CH3:9])[N:3]=1.C(OO)(=[O:12])C.[OH-].[K+]>C(O)(=O)C>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][CH3:9])[N+:3]=1[O-:12]参加物
5
反応条件
- 温度
- 50 °C
実験手順
To a solution of 2-bromo-6-ethyl-pyridine (15.4 g, 82.8 mmol) (S. G. Davies and M. R. Shipton, J. Chem. Soc., Perkin Trans. 1, 1991, 3, 501) in acetic acid (15 ml) was added peracetic acid (26 ml of a 39% solution) maintaining T<50° C. After complete addition the mixture was stirred at 50° C. for 5 hr and then cooled to room temperature (rt). Crushed ice (40 g) was added and the pH was adjusted to pH 12 with 40% aqueous KOH solution. After extraction with CHCl3 (6×60 ml) the combined organic phases were dried (Na2CO3) and evaporated to give 20.0 g (>100%) of the title compound, MS: m/e=201 (M+) as a yellow oil.
後処理
- additionAfter complete addition the mixture
- temperaturecooled to room temperature (rt)
- extractionAfter extraction with CHCl3 (6×60 ml) the combined organic phases
- dry with materialwere dried (Na2CO3)
- customevaporated
出典と根拠
- ORDレコード
- ord-5fc7d08271054fa6be5311bba638694d
- 出典データセット
- uspto-grants-2004_12
- 特許番号
- US06831087B2
反応ノート
読み込み中…