Reaktion #59649

ord-edc8959a3ec14e8e9a416f73ba49e7be

Reaktionsgleichung

C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23
levofloxacin
→
C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23.C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23.O
levofloxacin hemihydrate
Ausbeute 118.5%

Edukte

C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23
levofloxacin

Reagenzien

Keine

Lösungsmittel

CCCCO
n-BuOH

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was heated
  2. 2
    Temperaturto reflux temperature
  3. 3
    workup.DISSOLUTIONuntil complete dissolution of the material
  4. 4
    FiltrationThe precipitate was filtrated under vacuum
  5. 5
    Waschenwashed with n-BuOH
  6. 6
    Sonstigedried at 60° C. in a vacuum oven

Vorschrift

1 g of levofloxacin crude was put in suspension in 7 ml of n-BuOH. The mixture was heated to reflux temperature until complete dissolution of the material. Then the solution was cooled to RT over a period of 2.5 hours. The precipitate was filtrated under vacuum, washed with n-BuOH and dried at 60° C. in a vacuum oven to give 810 mg (81%) of purified levofloxacin hemihydrate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425628B2uspto-grants-2008_09