反応式
[Cl-].[Al+3].[Cl-].[Cl-].[C:5](OC(=O)C)(=[O:7])[CH3:6].[CH3:12][O:13][C:14]([C:16]1[CH:17]=[C:18]2[C:22](=[CH:23][CH:24]=1)[N:21]([S:25]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)(=[O:27])=[O:26])[CH:20]=[CH:19]2)=[O:15]>ClC(Cl)C>[CH3:12][O:13][C:14]([C:16]1[CH:17]=[C:18]2[C:22](=[CH:23][CH:24]=1)[N:21]([S:25]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)(=[O:26])=[O:27])[CH:20]=[C:19]2[C:5](=[O:7])[CH3:6])=[O:15]参加物
実験手順
To a suspension of 10.7 g (80 mmol) of aluminum chloride in dichloroethane (80 ml) was added dropwise 4.83 g (40 mmol) of acetic anhydride. After stirring for 15 min, to the mixture was added dropwise 6.31 g (20 mmol) of the above-mentioned 1-benzenesulfonylindole-5-carboxylic acid methyl ester in dichloroethane (60 ml). After stirring for 2 hours at room temperature, to the mixture were added 5.33 g (40 mmol) of aluminum chloride and 2.04 g (20 mmol) of acetic anhydride. After stirring for 30 min, the mixture was poured into ice-water, extracted with ethyl acetate. The extract was washed twice with water, aqueous sodium bicarbonate and dried, and then concentrated. The obtained crystal was washed with isopropyl ether to give 6.82 g of 3-acetyl-1-benzenesulfonylindole-5-carboxylic acid methyl ester. Yield: 96%.
後処理
- stirringAfter stirring for 2 hours at room temperature, to the mixture
- stirringAfter stirring for 30 min
- extractionextracted with ethyl acetate
- washThe extract was washed twice with water, aqueous sodium bicarbonate
- customdried
- concentrationconcentrated
- washThe obtained crystal was washed with isopropyl ether
出典と根拠
- ORDレコード
- ord-7988fd239167492c82cfcab229980e81
- 出典データセット
- uspto-grants-2001_12
- 特許番号
- US06333323B1
関連ノート
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