Sodium Hydroxide → 5-ethyl-6-nitro-2,3-dihydro-1H-indole
反応式
[CH2:1]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[NH:8][CH2:7][CH2:6]2)[CH3:2].[N+:12]([O-])([O-:14])=[O:13].[K+].[OH-].[Na+]>OS(O)(=O)=O>[CH2:1]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13])[NH:8][CH2:7][CH2:6]2)[CH3:2]参加物
5
反応条件
- 温度
- 5 °C
実験手順
To a solution of 5-ethylindoline (2.5 g, 17 mmol) in H2SO4 (98%, 20 mL) was slowly added KNO3 (1.7 g, 17 mmol) at 0° C. The mixture was stirred at 0-10° C. for 10 minutes. The mixture was then carefully poured into ice, basified with NaOH solution to pH 9, and extracted with ethyl acetate. The combined extracts were washed with brine, dried over Na2SO4 and concentrated to dryness. The residue was purified by silica column to give 5-ethyl-6-nitroindoline (1.9 g, 58%).
後処理
- customat 0° C
- additionThe mixture was then carefully poured into ice
- extractionextracted with ethyl acetate
- washThe combined extracts were washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated to dryness
- customThe residue was purified by silica column
出典と根拠
- ORDレコード
- ord-947e4326cc2344fb9ca585b4b9ae0a26
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08623905B2
反応ノート
読み込み中…