반응 #59652

반응 방정식

levofloxacin

levofloxacin

→

levofloxacin hemihydrate

수율 108.9%

용매

ACN H2O

—

mixture

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도to reflux during 1 hour
3. 3
   여과filtrated under vacuum with Hyflow when still hot
4. 4
   온도Then the solution was heated again
5. 5
   온도to reflux
6. 6
   여과The precipitate was filtrated under vacuum
7. 7
   세척washed with ACN
8. 8
   건조H2O (2×12 mL) and dried in a vacuum oven

실험 절차

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.

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