Bromine → HCID 58204120、化合物
反応式
[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]参加物
4
実験手順
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.
後処理
- customReaction
- concentrationConcentrated
- customthe reaction in vacuo
- custompurified by flash chromatography (0 to 30% ethyl acetate/heptanes)
- concentrationConcentrated in vacuo and NMR
出典と根拠
- ORDレコード
- ord-367f1565228c4a24b6cedeb19b317893
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08952043B2
反応ノート
読み込み中…