반응 #59651

반응 방정식

levofloxacin

sodium metabisulfite

→

levofloxacin hemihydrate

용매

n-BuOH H2O

—

mixture

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도to reflux temperature
3. 3
   workup.DISSOLUTIONuntil complete dissolution of the material
4. 4
   여과The precipitate was filtrated under vacuum
5. 5
   세척washed with a mixture n-BuOH:H2O (9:1) (4 ml)
6. 6
   기타dried at 60° C. in a vacuum oven

실험 절차

1.5 g of levofloxacin crude and 10 mg of sodium metabisulfite were put in suspension in 6 ml of a mixture n-BuOH:H2O (9:1) under nitrogen atmosphere. The mixture was heated to reflux temperature until complete dissolution of the material. Then the solution was cooled to RT over a period of 1.5 hours. The precipitate was filtrated under vacuum, washed with a mixture n-BuOH:H2O (9:1) (4 ml) and dried at 60° C. in a vacuum oven to give 1.2 g (81%) of purified levofloxacin hemihydrate. The purified levofloxacin hemihydrate contained virtually no N-oxide levofloxacin.

출처