反応式
[Cl:1][C:2]1[CH:26]=[CH:25][CH:24]=[CH:23][C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]2[S:15](=[O:17])(=[O:16])[CH2:14][CH2:13][C:12]([C:18]([O:20]C)=[O:19])=[CH:11][C:10]=2[CH:22]=1.C(=O)([O-])[O-].[K+].[K+].Cl>C1COCC1.CO>[Cl:1][C:2]1[CH:26]=[CH:25][CH:24]=[CH:23][C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]2[S:15](=[O:17])(=[O:16])[CH2:14][CH2:13][C:12]([C:18]([OH:20])=[O:19])=[CH:11][C:10]=2[CH:22]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 65 °C
実験手順
Into a solution of methyl 7-[(2-chlorobenzyl)oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (350 mg) in THF-methanol (7-3.5 ml) was added at room temperature a 2 M aqueous solution of potassium carbonate (0.9 mg), and the resulting mixture was stirred at 65° C. for 20 hours. After cooling to room temperature, the reaction mixture was mixed with 1 N hydrochloric acid (10 ml) and was extracted with ethyl acetate. The organic layer was washed with an aqueous saturated solution of sodium chloride and was dried with magnesium sulfate. After concentration under reduced pressure, the precipitated crystals were collected by filtration. The crystals were washed with diisopropyl ether to obtain 7-[(2-chlorobenzyl)oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (303 mg) as colorless crystals.
後処理
- temperatureAfter cooling to room temperature
- extractionwas extracted with ethyl acetate
- washThe organic layer was washed with an aqueous saturated solution of sodium chloride
- dry with materialwas dried with magnesium sulfate
- concentrationAfter concentration under reduced pressure
- filtrationthe precipitated crystals were collected by filtration
- washThe crystals were washed with diisopropyl ether
出典と根拠
- ORDレコード
- ord-36320599eb03470fad06c2795e004406
- 出典データセット
- uspto-grants-2003_09
- 特許番号
- US06627651B1
関連ノート
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