Reaktion #80282

ord-c317843f65ba47bebddd862b2745b9a7

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Sonstigewas returned to room temperature
  3. 3
    Extraktionextracted with ethyl acetate
  4. 4
    WaschenThe organic layer was washed with water
  5. 5
    Trocknendried over anhydrous magnesium sulfate
  6. 6
    SonstigeCrystals obtained by concentration under reduced pressure
  7. 7
    Waschenwere washed with isopropyl ether

Vorschrift

A mixture comprising 54.2 g of 4-allyloxycarbonyl-5-hydroxy-2-methylbenzofuran-3-carboxylic acid, 47 g of 4,6-dimethoxy-2-methylsulfonylpyridine and 65 g of potassium carbonate in 200 ml of N,N-dimethylformamide, was heated and stirred at 70° C. for two hours. The mixture was returned to room temperature, and then the reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous magnesium sulfate. Crystals obtained by concentration under reduced pressure, were washed with isopropyl ether to obtain 79.2 g (yield: 98%) of the desired compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05616537uspto-grants-1997_04