Reaktion #59650

Reaktionsgleichung

levofloxacin

ascorbic acid

→

levofloxacin hemihydrate

Lösungsmittel

n-BuOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated
2. 2
   Temperaturto reflux temperature
3. 3
   Filtrationa hot filtration
4. 4
   SonstigeThe solution was then evaporated to dryness and n-BuOH (10 ml)
5. 5
   workup.ADDITIONwas added
6. 6
   TemperaturThe mixture was heated
7. 7
   Temperaturto reflux until complete dissolution
8. 8
   FiltrationThe precipitate was filtrated under vacuum
9. 9
   Waschenwashed with n-BuOH (4 ml)
10. 10
    Sonstigedried at 60° C. in a vacuum oven

Vorschrift

1.5 g of levofloxacin crude and 36 mg of ascorbic acid were put in suspension in 9.5 ml of n-BuOH under inert atmosphere. The mixture was heated to reflux temperature and a hot filtration was performed. The solution was then evaporated to dryness and n-BuOH (10 ml) was added. The mixture was heated to reflux until complete dissolution and then cooled to RT over a period of 1.5 hour. The precipitate was filtrated under vacuum, washed with n-BuOH (4 ml) and dried at 60° C. in a vacuum oven to give 840 mg (56%) of purified levofloxacin hemihydrate.

Quelle