Bromine → HCID 58204120、化合物

HRID 1849441ノート

反応式

HRID 1849441 の反応式
[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

  1. customReaction
  2. concentrationConcentrated
  3. customthe reaction in vacuo
  4. custompurified by flash chromatography (0 to 30% ethyl acetate/heptanes)
  5. 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

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