Acetone → Cefotaxime Sodium

HRID 355528

Reaktionsgleichung

Reaktionsgleichung von HRID 355528
O.O.O.C([O-])(=O)C.[Na+:8].CC(C)=O.[CH3:13][C:14]([O:16][CH2:17][C:18]1[CH2:39][S:38][C@@H:21]2[C@H:22]([NH:25][C:26](/[C:28](/[C:32]3[N:36]=[C:35]([NH2:37])[S:34][CH:33]=3)=[N:29]\[O:30][CH3:31])=[O:27])[C:23](=[O:24])[N:20]2[C:19]=1[C:40]([OH:42])=[O:41])=[O:15]>O>[CH3:13][C:14]([O:16][CH2:17][C:18]1[CH2:39][S:38][C@@H:21]2[C@H:22]([NH:25][C:26](/[C:28](/[C:32]3[N:36]=[C:35]([NH2:37])[S:34][CH:33]=3)=[N:29]\[O:30][CH3:31])=[O:27])[C:23](=[O:24])[N:20]2[C:19]=1[C:40]([O-:42])=[O:41])=[O:15].[Na+:8]

Komponenten

5

Edukt 3

HCID 180AcetoneHCID 5742673CefotaximeHCID 23665404Sodium Acetate Trihydrate

Produkt 1

HCID 10695961Cefotaxime Sodium

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

6 g of sodium acetate trihydrate are dissolved in 20 ml of water. 40 ml of acetone and 20 g of cefotaxime in free acid form are added to the stirred solution. The mixture is cooled to 0°. A solution is obtained within 2 to 5 minutes. The solution is filtered through a filter bed and subsequently through a sterile filter. The filters are washed with a chilled mixture of 3 ml of water and 15 ml of acetone. The filtrate is seeded with 0.2 g of seed crystals (Claforan®) and warmed to 20°. The mixture is stirred for 60 minutes. The sodium salt of cefotaxime partially crystallises. In order to compete crystallisation, 300 ml of acetone are added dropwise within 3 hours, and stirring is effected for a further 30 minutes at 20°. The sodium salt of cefotaxime is separated off by filtration, washed with acetone and dried overnight in a vacuum drying chamber at 40° and for 1.5 hours in a stream of dry nitrogen gas at 70°. Crystalline sodium cefotaxime substantially in form of needles is obtained.

Aufarbeitung

  1. temperatureThe mixture is cooled to 0°
  2. customA solution is obtained within 2 to 5 minutes
  3. filtrationThe solution is filtered through a filter bed and subsequently through a sterile filter
  4. washThe filters are washed with a chilled mixture of 3 ml of water and 15 ml of acetone
  5. temperaturewarmed to 20°
  6. customThe sodium salt of cefotaxime partially crystallises
  7. customcrystallisation, 300 ml of acetone
  8. additionare added dropwise within 3 hours
  9. stirringstirring
  10. waitis effected for a further 30 minutes at 20°
  11. customThe sodium salt of cefotaxime is separated off by filtration
  12. washwashed with acetone
  13. customdried overnight in a vacuum
  14. customdrying chamber at 40°
  15. waitfor 1.5 hours in a stream of dry nitrogen gas at 70°

Quellen und Nachweise

ORD-Eintrag
ord-829dd3a3103b46ecb6d581b38ac63dc9
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05831086

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