Ethyl Acetate → 5-Bromo-4-methylpyridine-3-carbonitrile
반응식
Br[C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Br:9])[C:7]=1[CH3:8].[C:10]([Cu])#[N:11].CCOC(C)=O>CN(C=O)C>[Br:9][C:6]1[C:7]([CH3:8])=[C:2]([C:10]#[N:11])[CH:3]=[N:4][CH:5]=1참가 물질
5
실험 절차
A mixture of 3,5-dibromo-4-methylpyridine (16 g, 64 mmol) and CuCN (6.2 g, 69 mmol) in 150 mL of DMF was refluxed for 4 hours before cooled down. The reaction mixture was poured to 1 L of EtOAc with stirring and the precipitate was removed by filtration. The filtrate was washed with water, brine, dried over anhydrous Na2SO4 and concentrated. The residue was purified by column chromatography to afford 5-bromo-4-methylpyridine-3-carbonitrile.
후처리
- temperaturewas refluxed for 4 hours
- temperaturebefore cooled down
- customthe precipitate was removed by filtration
- washThe filtrate was washed with water, brine
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated
- customThe residue was purified by column chromatography
출처 및 근거
- ORD 기록
- ord-5de5469c8b0e4c90afecc837e125c4d2
- 출처 데이터셋
- uspto-grants-2015_12
- 특허 번호
- US09206199B2
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