Bromine → HCID 58204120, 화합물
반응식
[F:1][C:2]1[CH:13]=[CH:12][C:5]2[O:6][CH2:7][CH2:8][CH2:9][C:10](=[O:11])[C:4]=2[CH:3]=1.[Br:14]Br>CCOCC>[Br:14][CH:9]1[CH2:8][CH2:7][O:6][C:5]2[CH:12]=[CH:13][C:2]([F:1])=[CH:3][C:4]=2[C:10]1=[O:11]참가 물질
4
실험 절차
Dissolved 7-fluoro-3,4-dihydrobenzo[b]oxepin-5(2H)-one (1.58 g, 8.77 mmol) in 80 mL ether and added bromine (0.497 mL, 9.65 mmol) and allowed the reaction mixture to stir at room temperature 20 hours. Reaction was complete by LCMS. Concentrated the reaction in vacuo and purified by flash chromatography (0 to 30% ethyl acetate/heptanes). Concentrated in vacuo and NMR indicated 4-bromo-7-fluoro-3,4-dihydrobenzo[b]oxepin-5(2H)-one.
후처리
- customReaction
- concentrationConcentrated
- customthe reaction in vacuo
- custompurified by flash chromatography (0 to 30% ethyl acetate/heptanes)
- concentrationConcentrated in vacuo and NMR
출처 및 근거
- ORD 기록
- ord-a9b4a591bb67435894647ba172590f40
- 출처 데이터셋
- uspto-grants-2015_11
- 특허 번호
- US09175009B2
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