Hydrochloric Acid → 1-Bromo-2-chloro-3-methylbenzene
反応式
Cl.[Br:2][C:3]1[CH:8]=[CH:7][C:6](N)=[C:5]([CH3:10])[C:4]=1[Cl:11].N([O-])=O.[Na+]>CCO>[Br:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:10])[C:4]=1[Cl:11]参加物
5
反応条件
- 温度
- 70 °C
実験手順
Concentrated HCl was added to a solution of 4-bromo-3-chloro-2-methyl-phenylamine (4.98 g, 22.60 mmol) in EtOH. NaNO2 (3.00 g, 43.50 mmol) was added and the resulting mixture was heated to 70° C. for 2 hours. Ethanol was distilled off and the residue was purified by column chromatography using hexanes as the eluant to afford the title compound. Spectroscopic data: 1H NMR (300 MHz, CDCl3) δ 2.43 (s, 3H), 7.01 (t, J=7.91 Hz, 1H), 7.18 (d, J=7.62 Hz, 1H), 7.47 (d, J=7.91 Hz, 1H).
後処理
- distillationEthanol was distilled off
- customthe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-c3199ebd740742edacdf4e2861858c08
- 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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