Water → 1-(5-Bromopyridin-3-yl)propan-2-one
반응식
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:13]=1)[C:7](N(OC)C)=O.[CH2:14]([Mg]Cl)[CH3:15].[OH2:18]>C1COCC1>[Br:1][C:2]1[CH:13]=[C:6]([CH2:7][C:14](=[O:18])[CH3:15])[CH:5]=[N:4][CH:3]=1참가 물질
5
실험 절차
44 g (180 mmol) of 5-bromo-N-methoxy-N-methylnicotinamide are dissolved in 200 mL of THF and 60 mL (180 mmol) of ethylmagnesium chloride solution (3M in ethyl ether) are added dropwise. The reaction medium is stirred at room temperature for one hour, poured into water and extracted with ethyl acetate. The organic phase is separated out after settling, dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a column of silica eluted with a mixture of heptane and ethyl acetate (70/30). 4 g (11%) of 1-(5-bromo-3-pyridyl)propanone are collected.
후처리
- extractionextracted with ethyl acetate
- customThe organic phase is separated out
- dry with materialdried over magnesium sulphate
- customevaporated
- customThe residue obtained
- customis purified by chromatography on a column of silica
- washeluted with a mixture of heptane and ethyl acetate (70/30)
- custom4 g (11%) of 1-(5-bromo-3-pyridyl)propanone are collected
출처 및 근거
- ORD 기록
- ord-dca96e3537174ceca06c1decd22b94ce
- 출처 데이터셋
- uspto-grants-2004_03
- 특허 번호
- US06706725B1
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