Diethyl Ether → 1-(6-Fluoropyridin-3-yl)ethan-1-one
반응식
[F:1][C:2]1[CH:9]=[CH:8][C:5](C#N)=[CH:4][N:3]=1.C[Mg]Br.C(=O)(O)[O-].[Na+].CC[O:20][CH2:21][CH3:22]>C1COCC1>[F:1][C:2]1[N:3]=[CH:4][C:5]([C:21](=[O:20])[CH3:22])=[CH:8][CH:9]=1참가 물질
6
실험 절차
To a solution of 6-fluoronicotinonitrile (5.00 g, 41.0 mmol) in THF (50 mL) was added 1 N methylmagnesium bromide (16.4 mL, 49.1 mmol) in THF at 0° C. After addition, the mixture was warmed to ambient temperature and stirred at ambient temperature for 4 hours. Saturated sodium bicarbonate solution (50 mL) and ether (100 mL) were added. The organic layer was separated, washed with brine, dried (sodium sulfate), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (5:1 hexane/ethyl acetate) to give 1-(6-fluoropyridin-3-yl)ethanone (0.85 g, 14.9%) as solid.
후처리
- additionAfter addition
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried (sodium sulfate)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was purified by flash chromatography on silica gel (5:1 hexane/ethyl acetate)
출처 및 근거
- ORD 기록
- ord-7b9bfa6b3acb4225acadabaf78514a12
- 출처 데이터셋
- uspto-grants-2014_11
- 특허 번호
- US08889704B2
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