Reaktion #3722

Reaktionsgleichung

clavulanic acid

potassium 2-ethylhexanoate

ethyl acetate

sulfuric acid

→

potassium clavulanate

Ausbeute 73.0%

Lösungsmittel

methyl isobutyl ketone

methyl isobutyl ketone

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas slowly added in order
2. 2
   ExtraktionAfter extracting the said mixture
3. 3
   Sonstigethe extracts are separated
4. 4
   ExtraktionThe remaining aqueous solution was further extracted with 100 ml of the solvent mixture three times
5. 5
   workup.ADDITIONAnhydrous magnesium sulfate (10 g) and activated carbon(10 g) were added to the
6. 6
   Extraktioncombined extract
7. 7
   FiltrationThe mixture was suction-filtered through a filter
8. 8
   Waschenthe remaining material was washed with 50 ml of methyl isobutyl ketone
9. 9
   workup.ADDITIONwas slowly added to the
10. 10
    Extraktionsaid extract
11. 11
    workup.STIRRINGthe mixture was agitated at 5° C. for 2 hours
12. 12
    FiltrationThe crystalline product was filtered
13. 13
    workup.WAITslurried with acetone at the same temperature for 2 hours
14. 14
    SonstigeThe crystalline was dried in a vacuum desiccator (30° C.) for about 5 hours

Vorschrift

100 ml of the solvent mixture of ethyl acetate and methyl isobutyl ketone (4:1) already cooled to 5° C. was added to 100 ml of aqueous solution containing clavulanic acid (12 mg/ml). While agitating the mixture, 50% sulfuric acid was slowly added in order to control pH at 1.5. After extracting the said mixture, the extracts are separated. The remaining aqueous solution was further extracted with 100 ml of the solvent mixture three times. Anhydrous magnesium sulfate (10 g) and activated carbon(10 g) were added to the combined extract, and the resultant mixture was agitated at 5° C. for 30 minutes. The mixture was suction-filtered through a filter, and the remaining material was washed with 50 ml of methyl isobutyl ketone. A solution of potassium 2-ethylhexanoate (1.5 equivalent) dissolved in methyl isobutyl ketone was slowly added to the said extract, and the mixture was agitated at 5° C. for 2 hours. The crystalline product was filtered and slurried with acetone at the same temperature for 2 hours. The crystalline was dried in a vacuum desiccator (30° C.) for about 5 hours to obtain 1.07 g of potassium clavulanate (yield: 73%).

Quelle