tert-Octylamine → Potassium Clavulanate

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Reaction Steps

5.5 g of the tert.octylamine salt of clavulanic acid are dissolved in 55 ml of iso-butanol containing 3.0% of water at a temperature of about 35°. 2.1 g of potassium acetate are dissolved in 55 ml of iso-butanol containing 0.25 ml of water and 0.2 ml of acetic acid. 6.0 ml of the potassium acetate solution are added dropwise to the solution of the clavulanic acid. 0.32 g of active carbon (Norit CG 1) are added. The suspension is stirred for ca. 15 minutes, filtrated and the filter is washed with 20 ml of iso-butanol. The solution is cooled to ca. 10° and the remaining solution of potassium acetate prepared as described above is added slowly. The mixture is cooled to ca. 5° and stirred for ca. 2 hours. A precipitate is formed which is filtrated off, washed with 30 ml of acetone and dried for about 20 hours in vacuo at ca. 45°. Potassium clavulanate is obtained (confirmed by 1H-NMR).

Provenance & Evidence