Reaktion #156226

ord-216f17993b204565b8b69a733f2d9dec

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGThe mixture was stirred
  2. 2
    Sonstigethe precipitated insoluble matter was separated
  3. 3
    workup.DISSOLUTIONThe filtrate was dissolved in a mixture of ethyl acetate and methanol
  4. 4
    Sonstigean insoluble matter was removed by filtration
  5. 5
    Sonstigecondensed under reduced pressure
  6. 6
    Waschenthe residue was washed with ethyl acetate
  7. 7
    Sonstigedried

Vorschrift

N-Bromosuccinimide (1.3 g) was added to a DMF solution (15 ml) of 4-hydroxy quinoline (1.0 g) and the mixture was stirred at room temperature for 15 hours. A sodium hydrogencarbonate aqueous solution of 25% sodium sulfite was added to the mixture. The mixture was stirred and the precipitated insoluble matter was separated. The filtrate was dissolved in a mixture of ethyl acetate and methanol, and an insoluble matter was removed by filtration. The filtrate was condensed under reduced pressure, and the residue was washed with ethyl acetate and dried to give the title compound (1.1 g) as a white powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822453B2uspto-grants-2014_09