반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([F:14])([F:13])[F:12])=[CH:7][CH:6]=1)=O.[NH2:15][C:16]1[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][N:17]=1.C(=O)(O)[O-].[Na+]>C(O)C>[CH3:22][C:19]1[CH:20]=[CH:21][C:16]2[N:17]([CH:2]=[C:3]([C:5]3[CH:10]=[CH:9][C:8]([C:11]([F:14])([F:13])[F:12])=[CH:7][CH:6]=3)[N:15]=2)[CH:18]=1참가 물질
5
실험 절차
24 g (0.077 mole) of 1-bromo-2-(4-trifluoromethylphenyl)-2-ethanone, 8.4 g (0.077 mole) of 2-amino-5-methylpyridine and 13 g of sodium bicarbonate are mixed in 210 ml of 95% strength ethanol, and this suspension is heated under reflux until the evolution of gas has ceased. The solvent is then evaporated off under reduced pressure and the evaporation residue is taken up with water and dichloromethane. The organic phase is decanted and dried over magnesium sulphate, and the solvent is removed by evaporation under reduced pressure. The residue is purified by column chromatography.
후처리
- temperaturethis suspension is heated
- temperatureunder reflux until the evolution of gas
- customThe solvent is then evaporated off under reduced pressure
- customThe organic phase is decanted
- dry with materialdried over magnesium sulphate
- customthe solvent is removed by evaporation under reduced pressure
- customThe residue is purified by column chromatography
출처 및 근거
- ORD 기록
- ord-a4f089c2a14f4280abf7024273451486
- 출처 데이터셋
- uspto-grants-1988_08
- 특허 번호
- US04767755
연결된 노트
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