Reaktion #163545

ord-cffd98ecd0f34ad1a0c86bed52615424

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was refluxed
  2. 2
    workup.ADDITIONtreated with ice cold
  3. 3
    FiltrationThe mixture was filtered
  4. 4
    Extraktionthe filtrate was extracted with dichloromethane
  5. 5
    Trocknendried over anhydrous sodium sulfate
  6. 6
    Einengenconcentrated

Vorschrift

To 2 g (10.5 mM) of 1-ethyl-1,4-dihydroquinoxaline-2,3-dione in 20 ml of dichloroethane were added dropwise 3.16 g (11.0 mM) of POBr3. The reaction mixture was refluxed under stirring for 2 h and then treated with ice cold and an aqueous sodium carbonate solution. The mixture was filtered and the filtrate was extracted with dichloromethane, dried over anhydrous sodium sulfate and concentrated to give 1.4 g of 3-bromo-1-ethyl-quinoxalin-2(1H)-one as a yellow solid. Yield: 53%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08835634B2uspto-grants-2014_09