Bromine → HCID 58204120, Verbindung

HRID 1190721Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1190721
[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]

Komponenten

4

Edukt 2

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

Produkt 1

HCID 58204120HCID 58204120, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-3a637dfb8d8a4c83b3b5b7b0fea5a7c8
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08673952B2

Notizen zur Reaktion

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