Reaktion #80280

ord-0c82442a7e5e45618635df81d6ba9673

Lösungsmittel

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 sodium sulfate
  6. 6
    EinengenThen, it was concentrated under reduced pressure
  7. 7
    Waschenthe obtained crystals were thoroughly washed with isopropyl ether

Vorschrift

A mixture comprising 1.3 g of methyl 6-hydroxy-3-methyl-benzisoxazol-7-carboxylate, 1.4 g of 4,6-dimethoxy-2-methylsulfonylpyrimidine and 1 g of potassium carbonate in 20 ml of N,N-dimethylformamide, was heated and stirred at 70° C. for two hours. The mixture was returned to room temperature, poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. Then, it was concentrated under reduced pressure, and the obtained crystals were thoroughly washed with isopropyl ether to obtain 1.6 g (yield: 73%) of the desired compound.

Quelle

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