Bromine → HCID 58204120, Verbindung

HRID 708263Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 708263
[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-a9b4a591bb67435894647ba172590f40
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09175009B2

Notizen zur Reaktion

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