Reaktion #81612

ord-124031ecb21442b89a16ecd519315e68

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturunder reflux for 18 hours
  3. 3
    Temperaturthe mixture was heated
  4. 4
    Temperaturunder reflux for a further 20 hours
  5. 5
    Temperaturcooled
  6. 6
    Sonstigethe solution was evaporated to about 10 ml
  7. 7
    ExtraktionThe mixture was extracted several times with ethyl acetate
  8. 8
    Waschenthe combined extracts were washed with water
  9. 9
    Trocknendried (MgSO4)
  10. 10
    SonstigeEvaporation of the solvent

Vorschrift

A mixture of 3-[2-[(4-chlorophenyl)sulphonylamino]ethyl]-5-(4-fluorobenzoyl)benzenepropanoic acid (0.25 g) and potassium carbonate (0.212 g) in anhydrous methanol (5.0 ml) was heated under reflux for 18 hours. Additional potassium carbonate (0.212 g) was added and the mixture was heated under reflux for a further 20 hours and then cooled. Water (15 ml) was added and the solution was evaporated to about 10 ml and then acidified with 2N hydrochloric acid. The mixture was extracted several times with ethyl acetate and the combined extracts were washed with water and dried (MgSO4). Evaporation of the solvent gave the title compound as a glass (0.22 g). Found: C,60.25; H,4.92; N,2.51. C25H24ClNO6S requires C,59.81; H,4.82; N,2.79%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05618941uspto-grants-1997_04