Hydrogen Bromide → 5-Bromo-2-(bromomethyl)-1,3-difluorobenzene
反応式
[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH2:9]O)=[C:6]([F:8])[CH:7]=1.[BrH:12].O>C(O)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH2:9][Br:12])=[C:6]([F:8])[CH:7]=1参加物
5
実験手順
A solution of 5-Bromo-2-hydroxymethyl-1,3-difluoro-benzene (0.89 g, 4.0 mmol) and 30 wt % of hydrogen bromide in acetic acid was stirred at room temperature for 90 minutes before it was poured into 80 ml of water. The mixture was extracted with pentane (3×50 ml) and the combined organic layers were washed with water (3×20 ml), dried over MgSO4 and concentrated at low pressure to afford the desired product (10.0 g, 98% yield). 1H NMR (CDCl3) δ: 4.47 (s, 2H), 7.09–7.10 (m, 1H), 7.12–7.13 (m, 1H).
後処理
- extractionThe mixture was extracted with pentane (3×50 ml)
- washthe combined organic layers were washed with water (3×20 ml)
- dry with materialdried over MgSO4
- concentrationconcentrated at low pressure
出典と根拠
- ORDレコード
- ord-ba6e6e5c48cd4d03884cbd039f21ad81
- 出典データセット
- uspto-grants-2006_12
- 特許番号
- US07148226B2
反応ノート
読み込み中…