반응 #3722

반응 방정식

clavulanic acid

potassium 2-ethylhexanoate

ethyl acetate

sulfuric acid

→

potassium clavulanate

수율 73.0%

용매

methyl isobutyl ketone

methyl isobutyl ketone

반응 조건

후처리

1. 1
   workup.ADDITIONwas slowly added in order
2. 2
   추출After extracting the said mixture
3. 3
   기타the extracts are separated
4. 4
   추출The 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
   추출combined extract
7. 7
   여과The mixture was suction-filtered through a filter
8. 8
   세척the remaining material was washed with 50 ml of methyl isobutyl ketone
9. 9
   workup.ADDITIONwas slowly added to the
10. 10
    추출said extract
11. 11
    workup.STIRRINGthe mixture was agitated at 5° C. for 2 hours
12. 12
    여과The crystalline product was filtered
13. 13
    workup.WAITslurried with acetone at the same temperature for 2 hours
14. 14
    기타The crystalline was dried in a vacuum desiccator (30° C.) for about 5 hours

실험 절차

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%).

출처