Refining method of candesartan
A technology of candesartan and a refining method, which is applied to the refining field of intermediate candesartan, can solve the problems of high usage of organic solvent, difficulty in filtration of material and liquid, environmental waste of materials and the like, and achieves low usage of solvent, Excellent refining effect, easy filtering and drying effect
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Embodiment 1
[0026] Take 20 g of crude candesartan, add 200 mL of 2 mol / L sodium hydroxide and 20 mL of tetrahydrofuran, and stir to dissolve. After cooling down to 15°C, add glacial acetic acid dropwise, adjust the pH to 6.5, stir and crystallize, continue to cool down to 5°C, add glacial acetic acid dropwise, adjust the pH to 5.5, stir and crystallize for 1 hour, suction filter, and dry to obtain a solid The white product was 17.6 g, and the purity of candesartan (HPLC) was 97.6%.
Embodiment 2
[0028] Take 20 g of crude candesartan, add 160 mL of 2 mol / L sodium hydroxide and 40 mL of tetrahydrofuran, and stir to dissolve. After cooling down to 10°C, add glacial acetic acid dropwise, adjust the pH to 6.0, stir and crystallize, continue to cool down to 0°C, add glacial acetic acid dropwise, adjust the pH to 5.0, stir and crystallize for 1 hour, filter and dry to obtain a solid White product 16.7g, candesartan purity (HPLC) 98.2%.
Embodiment 3
[0030] Take 20 g of crude candesartan, add 100 mL of 2 mol / L potassium hydroxide and 30 mL of tetrahydrofuran, and stir to dissolve. After cooling down to 13°C, add glacial acetic acid dropwise, adjust the pH to 6.2, stir and crystallize, continue to cool down to 3°C, add glacial acetic acid dropwise, adjust the pH to 5.3, stir and crystallize for 2 hours, suction filter, and dry to obtain a solid The white product was 16.0 g, and the purity of candesartan (HPLC) was 97.3%.
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