Reaktion #2331739

Reaktionsgleichung

Levofloxacin

→

levofloxacin hemihydrate

Lösungsmittel

toluene chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONby mixing for about 30 min to 2 hrs
2. 2
   SonstigeRemoved the insolubles
3. 3
   Filtrationby filtration
4. 4
   workup.ADDITIONtreated the clear solution with carbon
5. 5
   workup.DISTILLATIONdistilled off the toluene-chloroform at temperature below 60° C
6. 6
   workup.ADDITIONIsopropanol is added to the mass, temperature
7. 7
   Temperaturis raised to 65° C. to 90° C.
8. 8
   workup.ADDITIONis added to the reaction mass at temperature of 60° C. to 90° C.
9. 9
   workup.ADDITIONmixed for about 5 min to 30 min
10. 10
    Temperaturcooled to 15° C. to about 35° C.
11. 11
    workup.ADDITIONmixed for about 30 min to 4 hrs
12. 12
    Sonstigeisolated
13. 13
    Sonstigedried at temperature of 45° C. to 85° C. preferably at 60° C. to 70° C.

Vorschrift

Levofloxacin crude is dissolved in mixture of toluene-chloroform at temperature of 20° C. to 40° C. by mixing for about 30 min to 2 hrs. Removed the insolubles by filtration, treated the clear solution with carbon and distilled off the toluene-chloroform at temperature below 60° C. Isopropanol is added to the mass, temperature is raised to 65° C. to 90° C., known quantity of water preferably to make-up the water content about 12% to about 20%, more selectively about 15% is added to the reaction mass at temperature of 60° C. to 90° C., mixed for about 5 min to 30 min, cooled to 15° C. to about 35° C., mixed for about 30 min to 4 hrs, isolated and dried at temperature of 45° C. to 85° C. preferably at 60° C. to 70° C. gives the levofloxacin hemihydrate.

Quelle