Water → 2-Bromo-4-(trifluoromethoxy)phenol
反応式
[F:1][C:2]([F:12])([F:11])[O:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.[Br:13]Br.ClCCl.O>C(Cl)(Cl)Cl>[Br:13][C:6]1[CH:5]=[C:4]([O:3][C:2]([F:11])([F:12])[F:1])[CH:9]=[CH:8][C:7]=1[OH:10]参加物
6
反応条件
- 温度
- 0 °C
実験手順
To a cooled (0° C.) solution of 4-trifluoromethoxyphenol (35.6 g, 0.2 mol) in chloroform (280 ml) was added dropwise a solution of bromine (32 g, 0.2 mol) in chloroform (50 ml). The solution was stirred at 0° C. for 1 hour and at room temperature for 2 hours. Dichloromethane (200 ml) and water (400 ml) ware added and the organic phase was washed further with water (400 ml), brine (200 ml) and dried (MgSO4). The solvent was removed and the residue was purified by distillation at reduced pressure to give the title compound. 1H NMR (250 MHz, CDCl3) δ 7.38 (1H, d, J=2.1 Hz), 7.13 (1H, dd, J=9.1, 2.1 Hz), 7.03 (1H, d, J=9.1 Hz), and 5.53 (1H, s).
後処理
- washthe organic phase was washed further with water (400 ml), brine (200 ml)
- dry with materialdried (MgSO4)
- customThe solvent was removed
- distillationthe residue was purified by distillation at reduced pressure
出典と根拠
- ORDレコード
- ord-cc5e1f9aca214d949d3e24baa86dae86
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05919781
反応ノート
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