Reaktion #59652

Reaktionsgleichung

levofloxacin

levofloxacin

→

levofloxacin hemihydrate

Ausbeute 108.9%

Lösungsmittel

ACN H2O

—

mixture

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated
2. 2
   Temperaturto reflux during 1 hour
3. 3
   Filtrationfiltrated under vacuum with Hyflow when still hot
4. 4
   TemperaturThen the solution was heated again
5. 5
   Temperaturto reflux
6. 6
   FiltrationThe precipitate was filtrated under vacuum
7. 7
   Waschenwashed with ACN
8. 8
   TrocknenH2O (2×12 mL) and dried in a vacuum oven

Vorschrift

25 g of wet levofloxacin crude (about 22.17 g or dry levofloxacin) was put in suspension in 225 mL of mixture ACN:H2O (99:1) under nitrogen atmosphere. The mixture was heated to reflux during 1 hour and then filtrated under vacuum with Hyflow when still hot. Then the solution was heated again to reflux and cooled to 0° C. over a period of 1 hour. The precipitate was filtrated under vacuum, washed with ACN:H2O (2×12 mL) and dried in a vacuum oven to give 18.6 g (84%) of purified levofloxacin hemihydrate. The purified levofloxacin hemihydrate contained approximately one-third less desmethyl levofloxacin than in the crude sample.

Quelle