Peracetic Acid → 2-Bromo-6-ethyl-pyridine 1-oxide
반응식
[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]참가 물질
5
반응 조건
- 온도
- 50 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-5fc7d08271054fa6be5311bba638694d
- 출처 데이터셋
- uspto-grants-2004_12
- 특허 번호
- US06831087B2
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