Water → 7-Bromo-1-methyl-1H-indole
反応式
[Br:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:10]=1[NH:9][CH:8]=[CH:7]2.[C:11]([O-])([O-])=O.[K+].[K+].CI.O>CN(C=O)C>[Br:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:10]=1[N:9]([CH3:11])[CH:8]=[CH:7]2参加物
6
実験手順
7-Bromoindole(0.37 g, 1.9 mmol) was dissolved in dry DMF. K2CO3 (0.52 g, 3.8 mmol) and methyliodide (0.13 mL, 2.08 mmol) were added. The reaction was stirred at room temperature for 5 days, after which H2O (20 mL) was added, the water phase was extracted with Et2O (3×20 mL), and the combined organic phases were washed with brine, dried (MgSO4), filtered and concentrated in vacuo. The crude product was purified by chromatography, eluent EtOAc:petroleum ether 1:20 to give 7-bromo-1-methylindole as a crystalline compound.
後処理
- extractionthe water phase was extracted with Et2O (3×20 mL)
- washthe combined organic phases were washed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe crude product was purified by chromatography, eluent EtOAc:petroleum ether 1:20
出典と根拠
- ORDレコード
- ord-6a6cc6f75170470bb4e4d880a3663fcf
- 出典データセット
- uspto-grants-2002_08
- 特許番号
- US06432962B1
反応ノート
読み込み中…