Synthesis method of cefalonium impurity B
A kind of technology of ceflonine and synthesis method, applied in the synthesis field of ceflonine impurity B
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Embodiment 1
[0029] Dissolve 10.0g of cefalotin sodium (23.9mmol 1.0eq) in 75ml of water, stir at room temperature to dissolve, add 75ml of methanol, cool down to -20~-25°C, add triethylamine (23.9mmol 1.0eq), at -20~ After reacting at -25°C for 1 hour, transfer to 20~25°C and add 6 N HCl to quench the reaction, and adjust the pH to 4.0. Methanol was rotary evaporated, extracted with DCM, and the aqueous phase was lyophilized to obtain 9.6 g of crude product. Take 9.6g of the crude product and add 100ml of water to dissolve it, add 100ml of acetone dropwise, stir at 0~5°C, add 200ml of EA dropwise, and flocculent precipitates gradually appear. -5~0°C, stirred and grown the crystal for 1 hour, then filtered and dried with suction to obtain 7.5g of impurity B with a purity of 95.0%.
Embodiment 2
[0031] Dissolve 10.0g of cefalotin sodium (23.9mmol 1.0eq) in 75ml of water, stir at room temperature to dissolve, add 75ml of methanol, cool down to -35~-40℃, add triethylamine (23.9mmol 1.0eq), at -35~ After reacting at -40°C for 1 hour, transfer to 20~25°C and add 6 N HCl to quench the reaction, and adjust the pH to 4.0. Methanol was rotary evaporated, extracted with DCM, and the aqueous phase was lyophilized to obtain 9.3 g of crude product. Take 9.3g of the crude product and add 100ml of water to dissolve it, add 100ml of acetone dropwise, stir at 0~5°C, add 200ml of EA dropwise, gradually a flocculent precipitate appears. -5~0°C, stirred and grown the crystal for 1 hour, and dried with suction to obtain 7.1g of impurity B with a purity of 95.5%.
Embodiment 3
[0033] Dissolve 10.0g of cefalotin sodium (23.9mmol 1.0eq) in 75ml of water, stir at room temperature to dissolve, add 75ml of methanol, cool down to -20~-25℃, add sodium bicarbonate (23.9mmol 1.0eq), at -20~ After reacting at -25°C for 1 hour, transfer to 20~25°C and add 6 N HCl to quench the reaction, and adjust the pH to 4.5. Methanol was rotary evaporated, extracted with DCM, and the aqueous phase was lyophilized to obtain 9.5 g of crude product. Take 9.5g of the crude product and add 100ml of water to dissolve it, add 100ml of acetone dropwise, stir at 0~5°C, add 200ml of EA dropwise, gradually a flocculent precipitate appears. -5~0°C, stirred and grown the crystal for 1 hour, filtered and dried with suction to obtain 7.2g of impurity B with a purity of 95.2%.
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