反応式
Br[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[Br:8][C:9]1[CH:14]=[C:13]([CH3:15])[C:12]([OH:16])=[C:11]([CH3:17])[CH:10]=1.C([O-])(=O)C.[K+].O>CN(C)C=O.C(OCC)(=O)C>[CH2:6]([O:5][C:3](=[O:4])[CH2:2][O:16][C:12]1[C:13]([CH3:15])=[CH:14][C:9]([Br:8])=[CH:10][C:11]=1[CH3:17])[CH3:7]参加物
7
反応条件
- 温度
- 80 °C
実験手順
Ethyl bromoacetate (0.662 mL) was added to a mixture of 4-bromo-2,6-dimethylphenol (1.0 g) and potassium acetate (1.031 g) in N,N-dimethylformamide (10 mL), and the mixture was stirred at 80° C. for 3 hrs. Water and ethyl acetate were added to the reaction mixture. The organic layer was separated, washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-hexane=1/10) to afford the title compound (1.29 g).
後処理
- customThe organic layer was separated
- washwashed with water and brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-hexane=1/10)
出典と根拠
- ORDレコード
- ord-25ea414057584b038524dd258874c7e8
- 出典データセット
- uspto-grants-2008_08
- 特許番号
- US07417169B2
関連ノート
読み込み中…