Hydrochloric Acid → 7-Bromochromone
反応式
Cl.[Br:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=[O:15])/[CH:10]=[CH:11]/N(C)C)=[C:5]([OH:16])[CH:4]=1>ClCCl>[Br:2][C:3]1[CH:4]=[C:5]2[C:6]([C:9](=[O:15])[CH:10]=[CH:11][O:16]2)=[CH:7][CH:8]=1参加物
4
実験手順
A solution of concentrated hydrochloric acid (30 mL) was added to a solution of (E)-1-(4-bromo-2-hydroxyphenyl)-3-(dimethylamino)prop-2-en-1-one (10.4 g, 38.5 mmol) in dichloromethane (250 mL). The mixture was heated at reflux for 30 minutes and cooled to room temperature. The aqueous phase was extracted with dichloromethane (20 mL). The combined organic phases were washed with saturated sodium bicarbonate (50 mL), dried over sodium sulfate and filtered. The solvent was removed under reduced pressure to yield 7-bromo-4H-chromen-4-one (8.7 g, 38.5 mol, 100%).
後処理
- temperatureThe mixture was heated
- temperatureat reflux for 30 minutes
- extractionThe aqueous phase was extracted with dichloromethane (20 mL)
- washThe combined organic phases were washed with saturated sodium bicarbonate (50 mL)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customThe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-7a1acb49fd9f44058ade568147b52fcd
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09156823B2
反応ノート
読み込み中…