Potassium bisulfate → 5-Bromo-1-(difluoromethyl)-1,2-dihydropyridin-2-one

HRID 2069843Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2069843
[Br:1][C:2]1[CH:3]=[CH:4]/[C:5](=N\C(=O)C)/[N:6]([CH:8]([F:10])[F:9])[CH:7]=1.[OH:15]S([O-])(=O)=O.[K+]>CC#N.O>[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[O:15])[N:6]([CH:8]([F:10])[F:9])[CH:7]=1

Komponenten

5

Edukt 2

HCID 516920Potassium bisulfateHCID 178474078HCID 178474078, Verbindung

Produkt 1

HCID 231159945-Bromo-1-(difluoromethyl)-1,2-dihydropyridin-2-oneAusbeute 52 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a stirred solution of the crude N-[5-Bromo-1-difluoromethyl-1H-pyridin-(2E)-ylidene]-acetamide (1 g) in 10 ml CH3CN was added 1% KHSO4 in water (10 ml). The reaction mixture was heated at reflux for 3 hrs. The reaction mixture was cooled down and the solvent was removed under reduced pressure. Without any workup this crude was purified by column chromatography using 10% ethyl acetate in hexane to get 5-Bromo-1-difluoromethyl-1H-pyridin-2-one (550 mg, 52%).

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 3 hrs
  3. temperatureThe reaction mixture was cooled down
  4. customthe solvent was removed under reduced pressure
  5. customWithout any workup this crude was purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-e8a9e79139db415489562e427fff2311
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08299077B2

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