The preparation method of clavulanic acid amine salt
A technology of clavulanate amine salt and clavulanic acid, which is applied in the field of preparation of clavulanate amine salt, can solve the problems of deepening the color of the material liquid, consumption of heat source, consumption of cold source, etc., so as to minimize the degree of degradation and improve product quality , the effect of improving product yield
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[0026] In the preparation of the clavulanic acid amine salt in the step (2), the clavulanic acid extraction concentrate obtained in the above step (1) is mixed with an organic amine donor and a co-solvent to obtain an insoluble clavulanic acid amine salt, which is filtered and drying to obtain clavulanic acid amine salt crystals.
[0027] Wherein, the co-solvent may be alcohol, such as methanol, ethanol, isopropanol or a mixture thereof, preferably methanol. During the mixing process in step (2), the volume ratio of the co-solvent to the clavulanic acid extraction concentrate is greater than or equal to 0.05 and less than or equal to 0.1.
[0028]The organic amine donor may be selected from n-butylamine, tert-butylamine, n-octylamine and tert-octylamine, preferably from tert-butylamine and tert-octylamine, and most preferably tert-butylamine. The organic amine donor is added in the form of a solution in any appropriate solvent system, preferably in the form of a solution in t...
Embodiment 1
[0031] Take 3 L of clavulanic acid aqueous solution (concentration 18.5 mg / mL, pH 5.10), control the temperature at 5 °C, adjust the pH to 1.60 with 25% sulfuric acid, add 19.8 g of ammonium sulfate, and after fully dissolving, add 2 times the volume of ethyl acetate ester, mixed well, and separated the light phase after standing to separate layers to obtain 5.9L of extract containing clavulanic acid (concentration 9.2mg / mL); then use organic solvent-resistant polyimide roll film (2,2 -Bis(3,4-dicarboxylic acid phenyl)hexafluoropropane dianhydride (6FDA), pyromellitic dianhydride (PMDA) and 4,4'-diaminodiphenyl ether (ODA) at a molar ratio of 0.5: 0.5:1 copolymer, the molecular weight cut-off is 600 Daltons) and concentrate the extract by nanofiltration to obtain clavulanic acid extract concentrate 0.82L (concentration 65.2mg / mL, color grade Y2);
[0032] At 5 °C, 41 mL of anhydrous methanol and the above clavulanic acid extract concentrate were added to a crystallization vess...
Embodiment 2
[0034] Take 3 L of clavulanic acid aqueous solution (concentration 19.7 mg / mL, pH 5.19), control the temperature at 5°C, adjust the pH to 1.30 with 25% sulfuric acid, add 19.8 g of ammonium sulfate, and after fully dissolving, add 3 times the volume of ethyl acetate ester, mixed thoroughly, and separated the light phase after standing to separate layers to obtain 8.8L of clavulanic acid extract (concentration 6.5mg / mL); then use an organic solvent-resistant roll film ( S600) Concentrate the extract by nanofiltration to obtain 0.8 L of clavulanic acid extract concentrate (concentration 71.5 mg / mL, color grade Y3);
[0035] At 5 °C, 80 mL of anhydrous methanol and the above clavulanic acid extract concentrate were added to a crystallization vessel, 359 mL of a 1M solution of tert-butylamine in ethyl acetate was added within 60 min, and the mixture was stirred at 5 °C for an additional 60 min. Minutes, the crystals were filtered, washed and dried to obtain white crystals with a ...
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