Phosphorus tribromide → 3-(Bromomethyl)-2,4-difluorophenol
反応式
[F:1][C:2]1[C:7]([CH2:8]O)=[C:6]([F:10])[CH:5]=[CH:4][C:3]=1[OH:11].P(Br)(Br)[Br:13]>C(OCC)C.ClCCl>[Br:13][CH2:8][C:7]1[C:2]([F:1])=[C:3]([OH:11])[CH:4]=[CH:5][C:6]=1[F:10]参加物
5
実験手順
To a stirred solution of 2,4-difluoro-3-(hydroxymethyl)phenol (step 1, 410 mg, 256 mmol) in diethyl ether (4 mL) and dichloromethane (1 mL) was added phosphorus tribromide (0.257 mL, 2.71 mmol) at 0° C. The mixture was stirred for 30 min, and then the mixture was poured onto ice-aqueous sodium bicarbonate. The mixture was extracted with ethyl acetate (200 mL), and the organic layer washed with water and brine, dried over magnesium sulfate and evaporated to afford 266 mg (47%) of the title compound as a colorless oil, which was used in the next step without purification:
後処理
- additionthe mixture was poured onto ice-aqueous sodium bicarbonate
- extractionThe mixture was extracted with ethyl acetate (200 mL)
- washthe organic layer washed with water and brine
- dry with materialdried over magnesium sulfate
- customevaporated
出典と根拠
- ORDレコード
- ord-9a64de11d1444a81b758acf607c3eebc
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07354925B2
反応ノート
読み込み中…