Bromine → HCID 58204120、化合物

HRID 1190721ノート

反応式

HRID 1190721 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

反応物 2

HCID 24408BromineHCID 122435647-Fluoro-3,4-dihydro-1-benzoxepin-5(2H)-one

生成物 1

HCID 58204120HCID 58204120、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

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-3a637dfb8d8a4c83b3b5b7b0fea5a7c8
出典データセット
uspto-grants-2014_03
特許番号
US08673952B2

反応ノート

読み込み中…