Реакция #3722

Уравнение реакции

clavulanic acid

potassium 2-ethylhexanoate

ethyl acetate

sulfuric acid

→

potassium clavulanate

Выход 73.0%

Растворители

methyl isobutyl ketone

methyl isobutyl ketone

Условия реакции

Обработка

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

Методика

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%).

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