Water → 1-(7-Bromobenzofuran-2-YL)ethanone
反応式
[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:4]([CH:5]=O)[C:3]=1[OH:10].Cl[CH2:12][C:13](=[O:15])[CH3:14].C([O-])([O-])=O.[Cs+].[Cs+].O>CN(C=O)C>[C:13]([C:14]1[O:10][C:3]2[C:2]([Br:1])=[CH:9][CH:8]=[CH:7][C:4]=2[CH:5]=1)(=[O:15])[CH3:12]参加物
6
反応条件
- 温度
- 60 °C
実験手順
A mixture of 5.0 g (24.9 mmol) of 3-bromo-salicylaldehyde, 3.0 g (32.3 mmol, 2.6 mL) of chloroacetone and 12 g (37.2 mmol) of Cs2CO3 in 30 mL of dry DMF was heated to 60° C. overnight. After cooling at room temperature, water (100 mL) was added and the mixture was extracted with ethyl acetate. The organic layer was dried over MgSO4 and the solvents were removed under reduced pressure. The crude product was directly recrystallized from hexane to afford 2-acetyl-7-bromo benzo[b]furan as a pale orange crystal.
後処理
- temperatureAfter cooling at room temperature
- extractionthe mixture was extracted with ethyl acetate
- dry with materialThe organic layer was dried over MgSO4
- customthe solvents were removed under reduced pressure
- customThe crude product was directly recrystallized from hexane
出典と根拠
- ORDレコード
- ord-cc08ec01fc8c49478f24411e700e8844
- 出典データセット
- uspto-grants-2008_03
- 特許番号
- US07348359B2
反応ノート
読み込み中…