Reaktion #43924

ord-b08931a08ded42a5a2441ecd19047add

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was heated
  2. 2
    Temperaturunder reflux for 2 hr
  3. 3
    Temperaturto cool
  4. 4
    Extraktionextracted with ethyl acetate
  5. 5
    WaschenThe extract was washed with saturated brine
  6. 6
    Trocknendried over anhydrous magnesium sulfate
  7. 7
    Einengenconcentrated under reduced pressure

Vorschrift

4-(Chloromethyl)-7-hydroxy-2H-chromen-2-one (10.9 g, 51.8 mmol) was dissolved in 1 M aqueous sodium hydroxide solution (500 mL), and the mixture was heated under reflux for 2 hr. The reaction mixture was allowed to cool, acidified with concentrated sulfuric acid, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give the title compound (8.27 g, yield 83%) as brown crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732626B2uspto-grants-2010_06