Phosphorus tribromide → 3-Bromo-5-(1-bromo-ethyl)-pyridine
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8](O)[CH3:9])[CH:5]=[N:6][CH:7]=1.P(Br)(Br)[Br:12].C([O-])(O)=O.[Na+]>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]([CH:8]([Br:12])[CH3:9])[CH:3]=1参加物
5
実験手順
1-(5-Bromo-pyridin-3-yl)-ethanol (1.5 g, 7.4 mmol) is dissolved in DCM (70 mL) and phosphorus tribromide (0.73 mL, 7.4 mmol) is added. The mixture is stirred for 4 hrs and saturated NaHCO3 aqueous solution is used to adjust the pH to about 7. The mixture is then extracted with DCM (3×50 mL). The organic layers are combined and concentrated to give the crude product. Purification by flash column chromatography affords 850 mg of 3-bromo-5-(1-bromo-ethyl)-pyridine.
後処理
- extractionThe mixture is then extracted with DCM (3×50 mL)
- concentrationconcentrated
- customto give the crude product
- customPurification by flash column chromatography
出典と根拠
- ORDレコード
- ord-9383dfed97ab407e94f8081299d2b03b
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181272B2
反応ノート
読み込み中…