Levofloxacin → Levofloxacin Hydrate

HRID 31372

Reaktionsgleichung

Reaktionsgleichung von HRID 31372
[CH3:1][C@@H:2]1[N:23]2[C:6]3[C:7]([C:19]([C:21]([C:24]([OH:26])=[O:25])=[CH:22]2)=[O:20])=[CH:8][C:9]([F:18])=[C:10]([N:11]2[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]2)[C:5]=3[O:4][CH2:3]1.[O:27]=C1O[C@H]([C@H](CO)O)C(O)=C1O>CCCCO>[CH3:1][C@@H:2]1[N:23]2[CH:22]=[C:21]([C:24]([OH:26])=[O:25])[C:19]([C:7]3=[CH:8][C:9]([F:18])=[C:10]([N:11]4[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]4)[C:5](=[C:6]23)[O:4][CH2:3]1)=[O:20].[CH3:1][C@@H:2]1[N:23]2[CH:22]=[C:21]([C:24]([OH:26])=[O:25])[C:19]([C:7]3=[CH:8][C:9]([F:18])=[C:10]([N:11]4[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]4)[C:5](=[C:6]23)[O:4][CH2:3]1)=[O:20].[OH2:27]

Komponenten

4

Edukt 2

HCID 149096LevofloxacinHCID 54670067L-Ascorbic Acid

Produkt 1

HCID 3033924Levofloxacin HydrateAusbeute 554,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux temperature
  3. filtrationa hot filtration
  4. customThe solution was then evaporated to dryness and n-BuOH (10 ml)
  5. additionwas added
  6. temperatureThe mixture was heated
  7. temperatureto reflux until complete dissolution
  8. filtrationThe precipitate was filtrated under vacuum
  9. washwashed with n-BuOH (4 ml)
  10. customdried at 60° C. in a vacuum oven

Quellen und Nachweise

ORD-Eintrag
ord-d8361376169140b3b78d7b01078148ce
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07425628B2

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