반응 #59650

ord-d8361376169140b3b78d7b01078148ce

시약

없음

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was heated
  2. 2
    온도to reflux temperature
  3. 3
    여과a hot filtration
  4. 4
    기타The solution was then evaporated to dryness and n-BuOH (10 ml)
  5. 5
    workup.ADDITIONwas added
  6. 6
    온도The mixture was heated
  7. 7
    온도to reflux until complete dissolution
  8. 8
    여과The precipitate was filtrated under vacuum
  9. 9
    세척washed with n-BuOH (4 ml)
  10. 10
    기타dried 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07425628B2uspto-grants-2008_09