Reaktion #1885

ord-058d1ba117d240a89d29098d17908733

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed for 1 hour
  2. 2
    Temperaturwhile heating
  3. 3
    workup.DISTILLATIONAfter the solvent was distilled off
  4. 4
    Extraktionextracted with ethyl acetate
  5. 5
    WaschenAfter the extract was washed with water
  6. 6
    Sonstigedried
  7. 7
    Sonstigethe solvent was removed

Vorschrift

A mixture of 4.7 g of 2-acetylamino-5-chloro-2',4',6'-trimethoxybenzophenone, 50 ml of 6N hydrochloric acid and 50 ml of ethanol was refluxed for 1 hour while heating. After the solvent was distilled off, the residue was basefied with an aqueous solution of sodium hydrogen carbonate and then extracted with ethyl acetate. After the extract was washed with water and dried, the solvent was removed, and the residue was subjected to silica gel column chromatography to yield 3.75 g of a crystal.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05726306uspto-grants-1998_03