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Esomeprazole magnesium dihydrate preparation method

A technology for esomeprazole magnesium dihydrate and esomeprazole magnesium trihydrate, applied in the field of chemical synthesis of pharmaceutical compositions, can solve the problems of toxic chlorinated solvents, low yield and the like, and achieve product crystal form Single, reproducible, easy-to-use results

Active Publication Date: 2013-07-24
SHANGHAI HUILUN BIOLOGICAL TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] US 10 / 267959 discloses a method for preparing esomeprazole magnesium dihydrate A crystal form by esomeprazole potassium salt, wherein a toxic chlorinated solvent is used, and the yield is low

Method used

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  • Esomeprazole magnesium dihydrate preparation method

Examples

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Embodiment 1

[0051] Embodiment 1 Preparation of esomeprazole magnesium trihydrate

[0052] In a 1L three-necked flask, esomeprazole potassium (76.8g, absolute content 85%, 170mmol) was dissolved in deionized water (300mL), magnesium sulfate heptahydrate (49.3g, 200mmol) was dissolved in deionized water (150 mL) was slowly added dropwise to the above solution, and reacted at 35° C. for 3 hours, and a large amount of solids were precipitated. Heating was stopped, the solid was filtered out, washed with water four times, and dried under vacuum at 40°C overnight. 62.0 g of esomeprazole trihydrate was obtained with a yield of 95%. After chromatographic analysis, the HPLC purity of the product was 99.90%, and the ee value was 99.80%. X-ray powder diffraction pattern see figure 1 .

Embodiment 2

[0053] The preparation of embodiment 2 esomeprazole magnesium dihydrate type A

[0054] In a 250 mL flask, esomeprazole trihydrate (11.5 g, 15 mmol) was suspended in anhydrous methanol (15 mL) and stirred for 30 minutes to obtain a clear solution. Stir at 25°C for 2 hours, add a mixed solution (75mL) of acetone and water (volume ratio 4:1) at 10°C, stir overnight at this temperature, and a large amount of solids precipitate out. The solid was filtered, washed twice with acetone, and dried under vacuum at 40°C for 10 hours. Obtained 10.2 g of esomeprazole dihydrate form A with a yield of 91%. After chromatographic analysis, the HPLC purity of the product was 99.98%, and the ee value was 99.94%. X-ray powder diffraction pattern see figure 2 .

Embodiment 3

[0055] The preparation of embodiment 3 esomeprazole magnesium dihydrate type A

[0056]In a 250 mL flask, esomeprazole trihydrate (11.5 g, 15 mmol) was suspended in anhydrous methanol (15 mL) and stirred for 30 minutes to obtain a clear solution. Stir at 45°C for 1 hour, add a mixed solution (60 mL) of acetone and water (volume ratio 3:1) at 10°C, stir overnight at this temperature, and a large amount of solid precipitates out. The solid was filtered, washed twice with acetone, and dried under vacuum at 20°C for 30 hours. 10.0 g of esomeprazole dihydrate type A was obtained with a yield of 89%. After chromatographic analysis, the HPLC purity of the product was 99.98%, and the ee value was 99.92%. X-ray powder diffraction pattern see figure 2 .

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Abstract

The invention relates to an esomeprazole magnesium dihydrate preparation method. The method comprises the following steps: dissolving an esomeprazole magnesium trihydrate in a single or mixed solvent, adding an adverse solvent, stirring for precipitating a solid, separating the solid, washing the solid, and drying the solid to obtain an esomeprazole magnesium dehydrate having an A crystal form. The method has the advantages of economy, simple operation, single product crystal form, and high repeatability, and is suitable for the industrialized production.

Description

technical field [0001] The invention belongs to the field of chemically synthesized pharmaceutical compositions and relates to the preparation of esomeprazole magnesium salt which can be used in pharmaceutical compositions. Background technique [0002] The chemical structure of Omeprazole is 5-methoxy-2-[[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]sulfoxide]-1H-benzene Bimidazole is a new class of anti-peptic ulcer drugs and proton pump inhibitors, developed by the Swedish Astra company, is the world's first clinical application of proton pump inhibitors (proton pump inhibitor, PPI). The S-enantiomer of omeprazole, namely (S)-omeprazole, has better safety and efficacy. In 2001, it became the first chiral proton pump inhibitor listed in the world. The generic name is Esomeprazole Esomeprazole, trade name Nexium. In recent years, the drug has been at the forefront of the world's best-selling drugs and has broad market prospects. Esomeprazole magnesium salt trihydrate is a li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12
Inventor 李文华秦继红
Owner SHANGHAI HUILUN BIOLOGICAL TECH CO LTD
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