Sulfuric Acid → 6-bromo-3-methyl-2,3-dihydro-1H-indol-2-one
반응식
Br[C:2]1[NH:3][C:4]2[C:9]([C:10]=1[CH3:11])=[CH:8][CH:7]=[C:6]([Br:12])[CH:5]=2.S(=O)(=O)(O)[OH:14].O1CCOCC1>O>[Br:12][C:6]1[CH:5]=[C:4]2[C:9]([CH:10]([CH3:11])[C:2](=[O:14])[NH:3]2)=[CH:8][CH:7]=1참가 물질
5
실험 절차
To 2,6-dibromo-3-methyl-1H-indole (15.7 g) were added 3N aqueous sulfuric acid solution (100 ml) and dioxane (100 ml), and the mixture was refluxed for 5 hours. After the reaction was complete, water was added to the reaction solution, and the mixture was extracted with ethyl acetate solution. This ethyl acetate solution was washed with water and an aqueous sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1) to give the title compound (11.2 g) as a brown crystal.
후처리
- temperaturethe mixture was refluxed for 5 hours
- extractionthe mixture was extracted with ethyl acetate solution
- washThis ethyl acetate solution was washed with water
- dry with materialan aqueous sodium chloride solution, dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1)
출처 및 근거
- ORD 기록
- ord-474388bb84784cf79d8cab36be1433f8
- 출처 데이터셋
- uspto-grants-2013_03
- 특허 번호
- US08389511B2
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