Reaktion #65342

ord-3ea0abcb70e04f30b066fe9ef4b33779

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationfiltered
  2. 2
    Sonstigeevaporated
  3. 3
    Sonstigeto remove methanol
  4. 4
    workup.DISSOLUTIONThe residue was dissolved
  5. 5
    workup.ADDITIONby adding 74.2 g of isopropyl alcohol
  6. 6
    workup.STIRRINGthe resulting solution was stirred for one hour at 20° to 25° C.
  7. 7
    Sonstigeto precipitate the solid product
  8. 8
    FiltrationThe resulting solid was filtered
  9. 9
    Waschenwashed with 24.7 g of isopropyl alcohol
  10. 10
    Sonstigedried in vacuum

Vorschrift

10 g of piroxicam was suspended in 83 g of methanol. To this suspension was added 1.95 g of 85% KOH at 15° to 20° C. The resulting solution was stirred for 30 minutes at the same temperature, filtered and evaporated to remove methanol. The residue was dissolved by adding 74.2 g of isopropyl alcohol and the resulting solution was stirred for one hour at 20° to 25° C. and then cooled to 0° C. to precipitate the solid product. The resulting solid was filtered, washed with 24.7 g of isopropyl alcohol and then dried in vacuum to obtain 9.4 g (Yield 84%) of piroxicam potassium.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05420124uspto-grants-1995_05