Reaktion #573179

ord-8566d3c36a1b400c91d2ee96d84d58da

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto react at 80° C. for one day
  2. 2
    TemperaturAfter cooling
  3. 3
    Extraktionthe reaction mixture was extracted with toluene
  4. 4
    Sonstigethe solvent was removed from the
  5. 5
    Extraktionextract
  6. 6
    Sonstigeto obtain 7.6 g of a crude product
  7. 7
    SonstigePurification by silica gel column chromatography

Vorschrift

In a reaction flask were charged 3.5 g of 5-[3-(S)-fluoroheptyloxy]-2-(4-hydroxyphenyl)pyrimidine synthesized in the same manner as in steps 1 to 7 of Example 1, 3.17 g of potassium carbonate, 70 ml of DMF, and 6.4 g of 2-(S)-tetrahydropyranyloxyheptyl tosylate in a nitrogen stream, and the mixture was allowed to react at 80° C. for one day. After cooling, water was added thereto, the reaction mixture was extracted with toluene, and the solvent was removed from the extract to obtain 7.6 g of a crude product. Purification by silica gel column chromatography gave 6.4 g of the titled compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05290477uspto-grants-1994_03