5-bromo-6-nitro-1H-indole → 5-Bromo-1H-indol-6-amine
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[N+:11]([O-])=O)[NH:7][CH:6]=[CH:5]2>C(O)C.[Ni]>[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[NH2:11])[NH:7][CH:6]=[CH:5]2参加物
4
実験手順
A mixture of 5-bromo-6-nitro-1H-indole (7.5 g, 31.1 mmol) and Raney Ni (1 g) in ethanol was stirred under H2 (1 atm) at room temperature for 2 h. The catalyst was filtered off and the filtrate was concentrated to dryness. The residue was purified by column chromatography on silica gel to give 5-bromo-1H-indol-6-ylamine (B-27) (2 g, 30%). 1H NMR (DMSO-d6) δ 10.6 (s, 1 H), 7.49 (s, 1 H), 6.79-7.02 (m, 1 H), 6.79 (s, 1 H), 6.14-6.16 (m, 1 H), 4.81 (s, 2 H).
後処理
- filtrationThe catalyst was filtered off
- concentrationthe filtrate was concentrated to dryness
- customThe residue was purified by column chromatography on silica gel
出典と根拠
- ORDレコード
- ord-a78875a20f6043eba5779623932f9bd2
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08629162B2
反応ノート
読み込み中…