A kind of refining method of high-purity ceftaroline axetil
A technology of ceftaroline fexetil and refining method, which is applied in the field of medicine, can solve the problems of undisclosed refining steps of ceftaroline fexaxil imidazolium salt, low purity and yield, difficult to meet the requirements of ceftaroline fexetil pharmacopoeia and industrial preparation requirements, and achieve The process operation is simple and easy, and the effect of high yield
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Embodiment 1
[0028] Add 10g crude ceftaroline benzimidazole salt to 35ml mixed solution (mixed solution is acetone and water, volume ratio 1:1), stir to dissolve, add dropwise methanol about 18ml at 30°C, dropwise rate 2ml / min, Turn on the stirring speed 10r / min and keep it for 1h, turn on the cooling, the cooling rate is 2℃ / h, and stop cooling when the temperature drops to -5℃, continue to stir for 4h, filter, the filter cake is soaked in 10ml methanol at -5℃, filtered under the conditions of room temperature In a tray with a thickness of 1 cm, dried under reduced pressure at 20°C for 5 hours to obtain 9.4 g of a refined product of ceftaroline proxetil benzimidazole salt, with a yield of 94% and a purity of 99.53% by high performance liquid chromatography.
Embodiment 2
[0030] Add 10g crude ceftaroline benzimidazole salt to 45ml mixed solution (mixed solution is acetone and water, volume ratio 1:1), stir to dissolve, add dropwise methanol about 22ml at 30°C at a rate of 2ml / min. Turn on the stirring speed 10r / min and keep it for 1h, turn on the cooling, the cooling rate is 2℃ / h, and stop cooling when it drops to 0℃, continue stirring for 4h, filter, soak the filter cake with 10ml methanol at 0℃, filter by suction, and spread it on the tray at room temperature With a medium thickness of 1 cm and drying under reduced pressure at 20°C for 5 hours, 9.3 g of a refined product of ceftaroline proxetil benzimidazole salt was obtained, with a yield of 93% and a purity of 99.78% by HPLC.
Embodiment 3
[0032] Add 100g crude ceftaroline benzimidazole salt to 400ml mixed solution (mixed solution is acetone and water, volume ratio 1:1), stir to dissolve, add 200ml methanol at 30°C, drop rate 20ml / min, turn on stirring Rotate speed 15r / min, start cooling after 1h, cooling rate is 2℃ / h, stop cooling when it drops to -5℃, keep stirring for 4h, filter, filter cake is soaked in 100ml methanol at -5℃, filtered, and spread on tray at room temperature With a medium thickness of 1 cm, dried under reduced pressure at 20° C. for 5 hours to obtain 94 g of a refined product of ceftaroline pivoxil benzimidazole salt with a yield of 94% and a purity of 99.83% by high performance liquid chromatography.
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