Azobisisobutyronitrile → 1-Bromo-3-(bromomethyl)-2-chlorobenzene
反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[Cl:9].C1C(=O)N([Br:17])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][Br:17])[C:3]=1[Cl:9]参加物
5
実験手順
A solution of 1-bromo-2-chloro-3-methyl-benzene (3.90 g, 19.00 mmol), NBS (3.60 g, 20.20 mmol) and a catalytic amount of AIBN (50 mg) in CCl4 was refluxed for 30 minutes. The reaction mixture was cooled to room temperature and filtered. The precipitate was washed with pentane. The solvent was distilled off and the residue was purified by column chromatography using pentane as the eluant to afford the title compound. Spectroscopic data: 1H NMR (300 MHz, CDCl3) δ 4.62 (s, 2H), 7.14 (t, J=7.62 Hz, 1H), 7.39 (dd, J=7.62 Hz, 1H), 7.60 (dd, J=7.91 Hz, 1H).
後処理
- filtrationfiltered
- washThe precipitate was washed with pentane
- distillationThe solvent was distilled off
- customthe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-769e8720fd494b18bcc6b7db6e6beb3c
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08557853B2
反応ノート
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