Sodium Iodide → 1-Chloro-2-(iodomethyl)benzene
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8]Br.[Na+].[I-:11]>CC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][I:11]参加物
4
実験手順
A mixture of 2-chlorophenylmethylbromide (4 g, 19.47 mmol) and NaI (14 g, 97.33 mmol) in acetone (40 ml) was stirred under reflux for 1 hour. The reaction mixture was cooled, filtered and concentrated in vacuo. The residue was triturated with hexane and filtered. The solution was concentrated in vacuo, and the resulting oil purified by flash chromatography (silica, hexane) to afford the title compound (4.67 g, 63%) as an oil: 1H NMR (CDCl3) δ 7.34 (4H, m), 4.54 (2H, s).
後処理
- temperatureunder reflux for 1 hour
- temperatureThe reaction mixture was cooled
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was triturated with hexane
- filtrationfiltered
- concentrationThe solution was concentrated in vacuo
- customthe resulting oil purified by flash chromatography (silica, hexane)
出典と根拠
- ORDレコード
- ord-3add077b7d2d471e92c369c89c8343fa
- 出典データセット
- uspto-grants-1999_12
- 特許番号
- US06008217
反応ノート
読み込み中…