반응 #59650
ord-d8361376169140b3b78d7b01078148ce
시약
없음
용매
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도The mixture was heated
- 2온도to reflux temperature
- 3여과a hot filtration
- 4기타The solution was then evaporated to dryness and n-BuOH (10 ml)
- 5workup.ADDITIONwas added
- 6온도The mixture was heated
- 7온도to reflux until complete dissolution
- 8여과The precipitate was filtrated under vacuum
- 9세척washed with n-BuOH (4 ml)
- 10기타dried at 60° C. in a vacuum oven
실험 절차
1.5 g of levofloxacin crude and 36 mg of ascorbic acid were put in suspension in 9.5 ml of n-BuOH under inert atmosphere. The mixture was heated to reflux temperature and a hot filtration was performed. The solution was then evaporated to dryness and n-BuOH (10 ml) was added. The mixture was heated to reflux until complete dissolution and then cooled to RT over a period of 1.5 hour. The precipitate was filtrated under vacuum, washed with n-BuOH (4 ml) and dried at 60° C. in a vacuum oven to give 840 mg (56%) of purified levofloxacin hemihydrate.