Реакция #59651

Уравнение реакции

levofloxacin

sodium metabisulfite

→

levofloxacin hemihydrate

Растворители

n-BuOH H2O

—

mixture

Условия реакции

Обработка

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

Методика

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.

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