Reaktion #59653

ord-f38215139cb6419da48d0bcd8cd9d6f6

Reaktionsgleichung

C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23
levofloxacin
O
H2O
→
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 84.0%

Edukte

C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23
levofloxacin
O
H2O

Reagenzien

Keine

Lösungsmittel

CS(C)=O
DMSO

Reaktionsbedingungen

Temperatur
108°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was cooled to RT
  2. 2
    FiltrationThe precipitate was filtrated under vacuum
  3. 3
    Waschenwashed with 1 ml of a mixture DMSO:H2O 1:5
  4. 4
    Sonstigedried at 60° C. in an air-flow oven

Vorschrift

1 g of levofloxacin crude was put in suspension in 1.5 ml of DMSO. The mixture was heated to 108° C. until complete dissolution of the material. Then H2O (7.5 ml) was added over 10 minutes and the mixture was cooled to RT. The precipitate was filtrated under vacuum, washed with 1 ml of a mixture DMSO:H2O 1:5 and dried at 60° C. in an air-flow oven to give 840 mg (84%) of purified levofloxacin hemihydrate.

Quelle

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