反应详情

温度

0 °C

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.

1. temperatureThe mixture was heated
2. temperatureto reflux during 1 hour
3. filtrationfiltrated under vacuum with Hyflow when still hot
4. temperatureThen the solution was heated again
5. temperatureto reflux
6. filtrationThe precipitate was filtrated under vacuum
7. washwashed with ACN
8. dry with materialH2O (2×12 mL) and dried in a vacuum oven