Method for refining esomeprazole sodium
A technology of esomeprazole sodium and its refining method, which is applied in the field of drug synthesis, can solve the problems of unqualified product quality, high cost, and environmental pollution caused by mixed component solvents, so as to reduce residues, reduce usage, and reduce pollution Effect
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Embodiment 1
[0026] The refining of embodiment 1 esomeprazole sodium:
[0027] Add 110 g of 7% sodium bicarbonate aqueous solution to the reaction bottle under nitrogen protection and light-shielding conditions, start stirring and add 50 g of crude esomeprazole sodium, add 80 ml of dichloromethane to the resulting reaction solution to extract non-polar impurities, and take the upper aqueous phase And add 50ml of ethanol and 3g of activated carbon and stir for 40 minutes, then filter with suction, and concentrate the filtrate under reduced pressure at 45°C until it becomes viscous, add 200ml of ethyl acetate to the residue, cool down to 5°C, stir and crystallize for 6 hours, and filter with suction , the filter cake was washed with cold ethyl acetate, and vacuum-dried at 35° C. for 7 hours to obtain 46.8 g of purified esomeprazole sodium white solid, with a refined yield of 93.5%. See Table 1 for the HPLC spectrum, Table 2 for the blank control spectrum, and Table 3 for the system suitabili...
Embodiment 2
[0028] The refining of embodiment 2 esomeprazole sodium:
[0029] Under nitrogen protection and shading conditions, add 100 g of 8.5% aqueous sodium bicarbonate solution to the reaction bottle, start stirring and add 50 g of crude esomeprazole sodium, add 90 ml of dichloromethane to the resulting reaction solution to extract non-polar impurities, and take the upper aqueous phase Add 60ml of ethanol and 4g of activated carbon and stir for 30 minutes, then filter with suction. The filtrate is concentrated under reduced pressure at 40°C until it becomes viscous. Add 250ml of ethyl acetate to the residue, cool down to 8°C, stir and crystallize for 5 hours, and filter with suction. , the filter cake was washed with cold ethyl acetate, and vacuum-dried at 35°C for 9 hours to obtain 46.2 g of purified white solid esomeprazole sodium, with a refined yield of 92.4%.
Embodiment 3
[0030] The refining of embodiment 3 esomeprazole sodium:
[0031] Under nitrogen protection and shading conditions, add 130g of 6% sodium bicarbonate aqueous solution to the reaction bottle, start stirring and add 50g of crude esomeprazole sodium, add 100ml of dichloromethane to the obtained reaction solution to extract non-polar impurities, and take the upper aqueous phase And add 50ml of ethanol, 2.5g of activated carbon and stir for 60 minutes, suction filtration, the filtrate is concentrated under reduced pressure at 50°C until it becomes viscous, 250ml of ethyl acetate is added to the residue, cooled to 5°C, stirred and crystallized for 4 hours, pumped After filtration, the filter cake was washed with cold ethyl acetate, and vacuum-dried at 40° C. for 7 hours to obtain 46.5 g of purified esomeprazole sodium white solid, with a refined yield of 93.0%.
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