Phosphorus tribromide → 4-Bromo-2-(bromomethyl)-1-fluorobenzene
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:10])=[C:6]([CH2:8]O)[CH:7]=1.P(Br)(Br)[Br:12].C([O-])(O)=O.[Na+]>COCCOC>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:10])=[C:6]([CH2:8][Br:12])[CH:7]=1参加物
5
実験手順
To (5-bromo-2-fluoro-phenyl)-methanol (1.2 g, 5.9 mmol) in DME (20 mL) was added phosphorus tribromide (0.83 mL, 8.8 mmol), and the reaction was stirred at room temperature for 6 hours. The mixture was cooled to 0° C. and adjusted to pH 6 with saturated aqueous NaHCO3. The solution was extracted with EtOAc, and the combined organic layers were dried, concentrated, and purified by silica gel chromatography to give the title compound.
後処理
- temperatureThe mixture was cooled to 0° C.
- extractionThe solution was extracted with EtOAc
- customthe combined organic layers were dried
- concentrationconcentrated
- custompurified by silica gel chromatography
出典と根拠
- ORDレコード
- ord-81d61cfb8f294986860eb236a730ea7e
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08067445B2
反応ノート
読み込み中…