2-Chloro-6-methylaniline → Benzenamine, 4-bromo-2-chloro-6-methyl-, hydrobromide (1:1)
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH2:9].[Br:10]Br>CO.C(O)(=O)C>[BrH:10].[Br:10][C:6]1[CH:5]=[C:4]([CH3:8])[C:3]([NH2:9])=[C:2]([Cl:1])[CH:7]=1参加物
5
実験手順
2-Chloro-6-methyl-phenylamine (5.00 g, 35.3 mmol) was dissolved in methanol (15 mL) and acetic acid was added (5 mL). The solution was chilled in an ice bath and a solution of bromine (1.8 mL) in acetic acid (15 mL) was added dropwise. After complete addition MeOH (5 mL) was added to dissolve the precipitated solid. The solvents were removed under reduced pressure and the residue was triturated with hexanes to provide the title compound as an off white solid (10.49 g, 99%). 1H NMR (300 MHz, MeOD): δ 7.42 (s, 1H), 7.28 (s, 1H), 2.42 (s, 3H).
後処理
- temperatureThe solution was chilled in an ice bath
- additionwas added
- dissolutionto dissolve the precipitated solid
- customThe solvents were removed under reduced pressure
- customthe residue was triturated with hexanes
出典と根拠
- ORDレコード
- ord-c561d30f7ee94b499f5cc000ff935faa
- 出典データセット
- uspto-grants-2011_06
- 特許番号
- US07968570B2
反応ノート
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