Reaktion #1154132

ord-6005579a6d87443e93a9a6702d5d0c98

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe organic phase is separated
  2. 2
    Sonstigedried
  3. 3
    Einengenconcentrated by evaporation

Vorschrift

72 mg of 6-(4-methyl4-phenyl-2-oxo-valeroylamino)-4-methyl-2,3-benzoxazin-1-one in 4 ml of tetrahydrofuran is mixed with 3 ml of methylmagnesium bromide (3 mol) at 0° C. After 30 minutes, ammonium chloride solution is added, the organic phase is separated, dried and concentrated by evaporation. After chromatography on silica gel (hexane/ethyl acetate 1:1), 39 mg of 6-(2-hydroxy-2,4-dimethyl4-phenyl-valeroylamino)-4-methyl-2,3-benzoxazin-1-one, melting point 173-175° C., is obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06245804B1uspto-grants-2001_06