Phosphorus tribromide → 4-(Bromomethyl)-2-chloro-3-methylbenzonitrile
反応式
[Cl:1][C:2]1[C:9]([CH3:10])=[C:8]([CH2:11]O)[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].P(Br)(Br)[Br:14]>C(Cl)Cl>[Br:14][CH2:11][C:8]1[CH:7]=[CH:6][C:3]([C:4]#[N:5])=[C:2]([Cl:1])[C:9]=1[CH3:10]参加物
4
反応条件
- 温度
- -15 °C
実験手順
To a solution of compound 7B (700 mg, 3.9 mmol) in CH2Cl2 (15 mL) was added PBr3 (5.8 mL, 5.8 mmol, 1N in CH2Cl2) at −15° C., and stirred at −15° C. for 3 hr. The reaction was slowly quenched with saturated NaHCO3 solution at −15° C. The organic layer was separated, dried over MgSO4, and concentrated. Purification by silica gel chromatography (0-10% EtOAc in hexanes) provide the title compound (270 mg) as a white powder.
後処理
- customThe reaction was slowly quenched with saturated NaHCO3 solution at −15° C
- customThe organic layer was separated
- dry with materialdried over MgSO4
- concentrationconcentrated
- customPurification by silica gel chromatography (0-10% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-a53eda7a21c6493b8351a35a680eae0b
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732480B2
反応ノート
読み込み中…