Water → 1-(Benzofuran-5-yl)ethanone
反応式
C(O[CH:4](OCC)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13](=[O:15])[CH3:14])=[CH:9][CH:8]=1)C.O>C1(C)C=CC=CC=1>[O:6]1[C:7]2[CH:12]=[CH:11][C:10]([C:13](=[O:15])[CH3:14])=[CH:9][C:8]=2[CH:4]=[CH:5]1参加物
4
実験手順
To a solution of 1-(4-(2,2-diethoxyethoxy)phenyl)ethanone (2.46 g, 7.34 mmol) in toluene (25 mL), was added PPA (2.50 g) and refluxed for 1 hour. Under ice-cold conditions, the reaction solution was added water, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate), and the title compound (44 mg (yield 3.7%)) was obtained as a white solid.
後処理
- temperaturerefluxed for 1 hour
- extractionextracted with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customThe obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate)
出典と根拠
- ORDレコード
- ord-45e55d23ac7c4ba6a904f03e879d7a20
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08551985B2
反応ノート
読み込み中…