Hydrochloric Acid → 7-Bromochromone
반응식
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]=1참가 물질
4
실험 절차
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%).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-7a1acb49fd9f44058ade568147b52fcd
- 출처 데이터셋
- uspto-grants-2015_10
- 특허 번호
- US09156823B2
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