Sulfuric Acid → 6-bromo-3-methyl-2,3-dihydro-1H-indol-2-one
反応式
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]=1参加物
5
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-474388bb84784cf79d8cab36be1433f8
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08389511B2
反応ノート
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