Phosphorus tribromide → 4-(bromomethyl)-2-methoxy-1-methylbenzene
反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[CH3:11])[CH2:6]O.P(Br)(Br)[Br:13]>CCOCC>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[CH3:11])[CH2:6][Br:13]参加物
4
反応条件
- 温度
- 0 °C
実験手順
A solution of 18.3 g (0.12 mol) of 3-methoxy4-methylbenzyl alcohol in 150 mL of Et2O was treated with 23.8 g (0.12 mol) of BaCO3 and the mixture cooled in ice. This was treated dropwise with 5.8 mL (0.06 mol) of PBr3. After stirring at 0° C. for 15 minutes, the mixture was allowed to stir at room temperature overnight. The mixture was filtered and the solid washed with Et2O. The Et2O was washed with saturated NaHCO3, then with saturated NaCl. Drying over MgSO4 and removal of the solvent under reduced pressure left 24.17 g (93.5% yield) of the product as an oil. The structure was confirmed by NMR spectroscopy.
後処理
- temperaturethe mixture cooled in ice
- stirringto stir at room temperature overnight
- filtrationThe mixture was filtered
- washthe solid washed with Et2O
- washThe Et2O was washed with saturated NaHCO3
- dry with materialDrying over MgSO4 and removal of the solvent under reduced pressure
出典と根拠
- ORDレコード
- ord-9ead9fca811340469570486b4764c12b
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06133303
反応ノート
読み込み中…