Reaktion #64273

Reaktionsgleichung

triethylamine

loracarbef

ethyl paraben

hydrochloric acid

→

Loracarbef DMF

Ausbeute 85.3%

Lösungsmittel

DMF

H2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto obtain a clear solution
2. 2
   Sonstigethe crystallization of the titled product
3. 3
   Filtrationfiltered
4. 4
   Waschenwashed with a solution of 10:1/DMF
5. 5
   TrocknenH2O, and dried under a vacuum at 40° C

Vorschrift

To a mixture of loracarbef: ethyl paraben (1.34 g, 65.5% potency as loracarbef) in 18 ml of DMF and 1.8 ml of H2O was added concentrated hydrochloric acid sufficient to obtain a clear solution. The pH of the solution was slowly raised to 6.9 with triethylamine, and the crystallization of the titled product occurred quickly. The mixture was stirred for 1 hour at room temperature, filtered, washed with a solution of 10:1/DMF:H2O, and dried under a vacuum at 40° C. HPLC analysis indicated that no ethyl paraben was present. The actual yield was 1.01 g, 73.9% potency as loracarbef, the theoretical yield was 0.87 g as loracarbef, and the percent yield was 85.3%.

Quelle