6-bromo-4-nitro-1H-indole → 4-Amino-6-bromoindole
반응식
[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[CH:7][NH:8]2)=[C:4]([N+:11]([O-])=O)[CH:3]=1>C(O)(=O)C.[Fe]>[Br:1][C:2]1[CH:3]=[C:4]([NH2:11])[C:5]2[CH:6]=[CH:7][NH:8][C:9]=2[CH:10]=1참가 물질
4
실험 절차
6-Bromo-4-nitro-1H-indole (1 g, 4.15 mmol) was treated with iron powder (1.16 g, 20 mmol) in acetic acid (60 ml) and stirred at room temperature. After 1 h the crude was filtered over Celite and the solvent was removed under reduced pressure. A mixture of a solution of sodium bicarbonate (4%) and ethyl acetate was added and the resulting mixture was filtered over Celite. The organic phase was washed with water and brine, dried over magnesium sulphate and the solvent was removed to give 1.05 g (100% yield) of the title compound as a dark solid, that was used in the next step without further purification. Purity 83%.
후처리
- filtrationAfter 1 h the crude was filtered over Celite
- customthe solvent was removed under reduced pressure
- additionA mixture of a solution of sodium bicarbonate (4%) and ethyl acetate
- additionwas added
- filtrationthe resulting mixture was filtered over Celite
- washThe organic phase was washed with water and brine
- dry with materialdried over magnesium sulphate
- customthe solvent was removed
출처 및 근거
- ORD 기록
- ord-0ff2c031d35f4db3aa1d6af2a331fb2b
- 출처 데이터셋
- uspto-grants-2016_07
- 특허 번호
- US09388189B2
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