Phosphorus tribromide → 1-(Bromomethyl)-3-chloro-2-methylbenzene
反応式
P(Br)(Br)[Br:2].[Cl:5][C:6]1[C:7]([CH3:14])=[C:8]([CH2:12]O)[CH:9]=[CH:10][CH:11]=1>C1(C)C=CC=CC=1>[Br:2][CH2:12][C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([Cl:5])[C:7]=1[CH3:14]参加物
4
実験手順
To a solution of phosphorus tribromide (0.422 mL, 4.47 mmol) in Toluene (30 mL) was added (3-chloro-2-methylphenyl)methanol (2 g, 12.77 mmol). The reaction was stirred at RT overnight. The solvent was removed and the residue was partitioned between EtOAc and brine. The organic layer was concentrated and the residue was purified by biotage (5% EA/hexane) to give the product (2.0 g, 71%). 1H NMR (400 MHz, CDCl3) δppm 7.36 (m, 1H), 7.24 (m, 1H), 7.12 (m, 1H), 4.56 (s, 2H). 2.48 (s, 3H).
後処理
- customThe solvent was removed
- customthe residue was partitioned between EtOAc and brine
- concentrationThe organic layer was concentrated
- customthe residue was purified by biotage (5% EA/hexane)
出典と根拠
- ORDレコード
- ord-bb8c0663e90045979d612542183e75cd
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08410095B2
反応ノート
読み込み中…