Water → 1-(5-Bromopyridin-3-yl)propan-2-one
反応式
[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]=1参加物
5
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-dca96e3537174ceca06c1decd22b94ce
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06706725B1
反応ノート
読み込み中…