Reaktion #64272

Reaktionsgleichung

loracarbef monohydrate

loracarbef monohydrate

Ethyl p-hydroxybenzoate

HCl

→

loracarbef

Ausbeute 98.2%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprecipitation
2. 2
   Sonstigeresulting in white crystals
3. 3
   Filtrationfiltered
4. 4
   Waschenwashed with H2O
5. 5
   Sonstigedried under vacuum at 40° C

Vorschrift

The pH of aqueous loracarbef monohydrate mother liquor (1000 ml, having 9.23 mg/ml of loracarbef monohydrate) was adjusted to 3.6 with HCl. Ethyl p-hydroxybenzoate (ethyl paraben) (4.52g) in ethanol (36 ml) was added dropwise over 15 minutes. After approximately 5 minutes, precipitation occurred, resulting in white crystals. The mixture was stirred overnight (15 hrs) at room temperature, filtered, washed with H2O, and dried under vacuum at 40° C. The yield was 11.72 g having a potency of 73.5% as loracarbef, and the theoretical yield was 8.78 g as loracarbef, resulting in a percent yield of 98.2%. The loracarbef:ethyl paraben exhibited the following X-ray powder diffraction pattern:

Quelle