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Refining method of sodium esomeprazole

A technology of esomeprazole sodium and its refining method, which is applied in the field of medicine and chemical industry, can solve the problems of low solubility, dark color, inability to effectively remove impurities, etc., and achieve the effect of low cost and high product purity

Active Publication Date: 2014-07-02
LUNAN BETTER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In international patent WO03 / 089408, simply use acetone as solvent refining esomeprazole sodium, add 0.7% sodium chloride solution simultaneously to remove impurity sulfone, but acetone is less to the dissolubility of esomeprazole sodium, this In the refining process of the traditional method, esomeprazole sodium is not completely dissolved all the time, and impurities cannot be effectively removed. The sulfone in the product is only <0.2%, and even the secondary refining cannot reduce the sulfone to below 0.1%. darker in color

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In a 1000 mL three-necked round bottom flask, 50.0 g of crude esomeprazole sodium was added (HPLC: 98.9%, sulfone: 0.6%, ee%: 99.4%). , Add a mixed solvent of methanol 50ml and acetone 250ml, stir and heat, reflux for 0.5h to completely dissolve the solids, cool slightly, add 1.0g of activated carbon, stir and reflux for 30min, filter while hot, slowly cool the filtrate to 35~45℃, add seed crystals, Stir and cool to 0~10℃ to crystallize for 6 hours, filter, wash the filter cake with acetone 50mL×2, and dry the filter cake under vacuum at 35~45℃ / -0.095MPa for 12 hours to obtain 42.7g of esomeprazole sodium. Refined yield :85.4%, HPLC: 99.9%, sulfone: 0.06%, ee%: 99.8%, the quality complies with the import standard of esomeprazole sodium JX20080210.

Embodiment 2

[0026] In a 2000mL three-necked round bottom flask, add 50.0g of crude esomeprazole sodium (HPLC: 98.7%, sulfone: 0.7%, ee%: 99.4%), add a mixed solvent of methanol 50mL and acetone 750ml, stir and heat, Reflux for 1.5h to fully dissolve the solids, cool slightly, add 1.0g of activated carbon, stir and reflux for 30min, filter while hot, slowly cool the filtrate to 35~45℃, add seed crystals, stir and cool to -10~0℃ to crystallize for 5 hours, filter The filter cake was washed with acetone 50mL×2, and the filter cake was vacuum-dried at 35~45℃ / -0.095MPa for 12 hours to obtain 43.1g of esomeprazole sodium. Refining yield: 86.2%, HPLC: 99.8%, sulfone: 0.05% , Ee%: 99.7%, the quality meets the import standard of esomeprazole sodium JX20080210.

Embodiment 3

[0028] In a 2000mL three-necked round bottom flask, add 50.0g crude esomeprazole sodium (HPLC: 99.0%, sulfone: 0.4%, ee%: 99.5%), add a mixed solvent of methanol 50mL and acetone 500ml, stir and heat, Reflux for 2.5h to dissolve the solids, cool slightly, add 1.0g of activated carbon, stir and reflux for 30min, filter while hot, slowly cool the filtrate to 35~45℃, add seed crystals, stir and cool to 0~10℃ to crystallize for 6 hours, filter, The filter cake was washed with acetone 50mL×2, and the filter cake was vacuum dried at 35~45°C / -0.095MPa for 12 hours to obtain 44.0g of esomeprazole sodium. Refined yield: 88.0%, HPLC: 99.9%, sulfone: 0.06%, ee%: 99.9%, the quality meets the import standard of esomeprazole sodium JX20080210.

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Abstract

The invention discloses a refining method of a sodium esomeprazole crude product by adopting a mixed solvent re-crystallization method. The method is simple and convenient to operate, high in product purity, low in content of a single impurity (the content of sulphone is less than 0.1 percent), high in yield, and more suitable for industrially largely producing the sodium esomeprazole.

Description

Technical field [0001] The invention belongs to the technical field of medicine and chemical engineering, and specifically relates to a method for refining esomeprazole sodium. Background technique [0002] Esomeprazole sodium, chemical name S-5-methoxy-2-{[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl] sub Sulfonyl}-1H-benzimidazole sodium is the first single enantiomer S-(-)-omeprazole sodium of the proton pump inhibitor omeprazole developed by AstraZeneca. salt. This medicine is mainly used for the treatment of gastric ulcer, duodenal ulcer, peptic esophagitis and gastritis. Compared with omeprazole, this product has a strong and long-lasting acid inhibitory effect, and also has a certain protective effect on the gastric mucosa. It is currently the first choice for the treatment of gastric acid-related diseases. Many literatures at home and abroad have reported its preparation methods, but there are few literatures related to specific purification methods. [0003] In the interna...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 赵志全郭彦玲田萌萌翟来生
Owner LUNAN BETTER PHARMA
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