Water → Ceftiofur

HRID 863651

Reaktionsgleichung

Reaktionsgleichung von HRID 863651
[CH3:1][O:2]/[N:3]=[C:4](\[C:11]([NH:13][C@@H:14]1[C:17](=[O:18])[N:16]2[C:19]([C:32]([OH:34])=[O:33])=[C:20]([CH2:23][S:24][C:25]([C:27]3[O:31][CH:30]=[CH:29][CH:28]=3)=[O:26])[CH2:21][S:22][C@H:15]12)=[O:12])/[C:5]1[N:9]=[C:8]([NH2:10])[S:7][CH:6]=1.Cl.O>O1CCCC1>[CH3:1][O:2]/[N:3]=[C:4](\[C:11]([NH:13][C@@H:14]1[C:17](=[O:18])[N:16]2[C:19]([C:32]([OH:34])=[O:33])=[C:20]([CH2:23][S:24][C:25]([C:27]3[O:31][CH:30]=[CH:29][CH:28]=3)=[O:26])[CH2:21][S:22][C@H:15]12)=[O:12])/[C:5]1[N:9]=[C:8]([NH2:10])[S:7][CH:6]=1

Komponenten

4

Edukt 2

HCID 962WaterHCID 9937686Ceftiofur Hydrochloride

Produkt 1

HCID 6328657CeftiofurAusbeute 84,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

Ceftiofur hydrochloride (17.1 g) is slurried for at least one hour at room temperature with 70 ml of tetrahydrofuran and 5.1 ml of water. To this slurry are added 8.6 g of PVP resin followed by 60 ml of tetrahydrofuran. After stirring for 45 minutes this slurry is filtered. The PVP resin is washed with two 31 ml portions of tetrahydrofuran. The filtrate is then added slowly over a period of about one hour to 515 ml of water at 45°-55° C. This slurry is stirred at 45°-55° C. for 30 minutes and filtered immediately at the end of the addition. The solids are washed with 70 ml of water and dried at 50° C. to give 13.5 g of crystalline ceftiofur free acid.

Aufarbeitung

  1. additionTo this slurry are added 8.6 g of PVP resin
  2. filtrationis filtered
  3. washThe PVP resin is washed with two 31 ml portions of tetrahydrofuran
  4. additionThe filtrate is then added slowly over a period of about one hour to 515 ml of water at 45°-55° C
  5. stirringThis slurry is stirred at 45°-55° C. for 30 minutes
  6. filtrationfiltered immediately at the end of the addition
  7. washThe solids are washed with 70 ml of water
  8. customdried at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-294a28bd957e460ab232035f87867f3f
Quelldatensatz
uspto-grants-1998_02
Patentnummer
US05721359

Verknüpfte Notizen

Wird geladen…