Reaktion #453503

ord-48695a53616e4648996b416b99881887

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter completion of the reaction
  2. 2
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure
  3. 3
    SonstigeThe obtained residue was purified directly by silica gel column chromatography

Vorschrift

20 ml of methanol was added to 0.4 g (1 mmol) of 3-(2-acetyl-4-chloro-6-fluorobenzofuran-7-yl) -1-methyl-6-trifluoromethyluracil, 0.4 g (4 mmol) of potassium acetate and 0.33 g (4 mmol) of methoxyamine hydrochloride, followed by stirring at room temperature for 12 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. The obtained residue was purified directly by silica gel column chromatography to obtain 0.28 g (yield: 64.6%) of the desired product as white powder. Melting point: 176-178° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06130187uspto-grants-2000_10