Sulfuric Acid → 1-(4-Fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid
반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[C:10]([C:15]#N)[C:9]2=[O:17])=[CH:4][CH:3]=1.[OH-:18].[Na+].S(=O)(=O)(O)[OH:21]>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[C:10]([C:15]([OH:21])=[O:18])[C:9]2=[O:17])=[CH:4][CH:3]=1참가 물질
반응 조건
- 온도
- 120 °C
실험 절차
1-(4-Fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile (3 g, 13.1 mmol) was dissolved in conc. sulfuric acid (6.0 mL) and water (6.0 mL), and the mixture was stirred with heating at 120° C. for 20 hr. 8N Aqueous sodium hydroxide solution was added to the reaction solution, and the mixture was washed with ethyl acetate. 2N hydrochloric acid was added to the aqueous layer, and the mixture was extracted twice with ethyl acetate. The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated under reduced pressure. The residue was washed with diethyl ether and collected by filtration to give the title compound (2.41 g, 74%) as a pale-brown solid.
후처리
- washthe mixture was washed with ethyl acetate
- addition2N hydrochloric acid was added to the aqueous layer
- extractionthe mixture was extracted twice with ethyl acetate
- washThe combined organic layer was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customthe solvent was evaporated under reduced pressure
- washThe residue was washed with diethyl ether
- filtrationcollected by filtration
출처 및 근거
- ORD 기록
- ord-7627c377691946cc8cd2cc8db824111b
- 출처 데이터셋
- uspto-grants-2013_05
- 특허 번호
- US08445509B2
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