High-purity sodium rabeprazole compound

A technology of rabeprazole sodium and rabeprazole, which is applied in the field of medicine, can solve the problems of destroying rabeprazole sodium, difficult to separate and the like, and achieves the effects of low toxicity, easy operation and simple method

Inactive Publication Date: 2012-05-09
HAINAN MEILAN SMITH KLINE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, adding strong acids such as HCl easily leads to destruction of rabeprazole sodium, and the solid acid salt of the present invention is acidified to avoid the degradation of rabeprazole sodium. Alkali is added to form a salt, which overcomes the disadvantages that impurities are easily brought in when the crude product of rabeprazole sodium is purified, and it is not easy to separate, so the pure product of rabeprazole sodium can be obtained with high yield and high purity

Method used

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  • High-purity sodium rabeprazole compound
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  • High-purity sodium rabeprazole compound

Examples

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Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 Refining of Rabeprazole Sodium

[0039] (1) 100g of rabeprazole and 12.5g of sodium hydroxide are stirred and reacted in water for 2 hours, and spray dried to generate 104.3g of rabeprazole sodium;

[0040] (2) Dissolve 100 g of the crude rabeprazole sodium in 2000 ml of water, add 20% sodium dihydrogen phosphate solution to adjust the pH to 5.5, stir to precipitate insoluble matter, filter, and wash with 200 ml of purified water to obtain a solid;

[0041] (3) Dissolve the solid obtained in step (2) with a mixture of 1500ml of dichloromethane and ethanol (1:4), adsorb it on D101 macroporous adsorption resin, and elute and purify it with 500ml of a mixture of chloroform and acetone (3:2). Collect the eluate;

[0042] (4) Adjust the pH value of the eluate obtained in step (3) to 9.0 with 5% sodium bicarbonate solution, precipitate solids, centrifuge for 10 minutes, wash with 200ml ethanol, and dry in vacuum at 40°C for 8 hours to obtain rabeprazole The pure sodium pro...

Embodiment 2

[0043] Example 2 Refining of Rabeprazole Sodium

[0044] (1) 100g rabeprazole and 12.8g sodium hydroxide are stirred and reacted in water for 2 hours, freeze-dried to generate 103.8g rabeprazole sodium;

[0045] (2) Dissolve 100 g of the crude rabeprazole sodium in 2000 ml of water, add 5% sodium hydrogen sulfate solution to adjust the pH to 7.5, stir to precipitate insoluble matter, filter, and wash with 200 ml of purified water to obtain a solid;

[0046] (3) Dissolve the solid obtained in step (2) with a mixture of 1500ml of dichloromethane and ethanol (1:4), adsorb it on AB-8 macroporous resin, and elute and purify it with 500ml of a mixture of chloroform and acetone (3:2) , Collect the eluate;

[0047] (4) Adjust the pH value of the eluate obtained in step (3) to 11.0 with 10% potassium bicarbonate solution, precipitate solids, centrifuge for 10 minutes, wash with 200ml ethanol, and dry under vacuum at 50°C for 5 hours to obtain rabeprazole The pure sodium product is 92.1g, the...

Embodiment 3

[0048] Example 3 Refining of Rabeprazole Sodium

[0049] (1) 100g of rabeprazole and 13.2g of sodium hydroxide were stirred and reacted in water for 2 hours, and spray dried to generate 105.1g of rabeprazole sodium;

[0050] (2) Dissolve 100 g of the crude rabeprazole sodium in 2000 ml of water, add 5% potassium hydrogen tartrate solution to adjust the pH to 6.8, stir to precipitate insoluble matter, filter, and wash with 200 ml of purified water to obtain a solid;

[0051] (3) Dissolve the solid obtained in step (2) with a mixture of 1500ml of dichloromethane and ethanol (1:4), adsorb it on AB-8 macroporous resin, and elute and purify it with 500ml of a mixture of chloroform and acetone (3:2) , Collect the eluate;

[0052] (4) Adjust the pH value of the eluate obtained in step (3) to 10.0 with 5% potassium carbonate solution, precipitate solids, centrifuge for 10 minutes, wash with 200ml ethanol, and vacuum dry at 45°C for 6 hours to obtain rabeprazole sodium The pure product is 9...

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PUM

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Abstract

The invention relates to a high-purity sodium rabeprazole compound, belonging to the technical field of medicine. The method includes the following steps: dissolving crude sodium rabeprazole synthesized by the reaction of rabeprazole and sodium hydroxide in water, adjusting pH value to be faintly acid to neutral by using solid acid salt, and collecting precipitated solid; after dissolving the solid with organic solvent, conducting elution and purification by using eluting agent through macroporous adsorption resin, and collecting eluent; and adjusting the pH value of the eluent to be alkaline, and collecting the precipitated solid to obtain the pure sodium rabeprazole.

Description

Technical field [0001] The invention relates to a high-purity rabeprazole sodium compound, which belongs to the technical field of medicine. Background technique [0002] Rabeprazole sodium, its chemical name is: 2-{[4-(3-methoxypropoxy)-3-methylpyridin-2-yl]methanesulfinyl}-1H-benzimidazole sodium , Molecular formula: C 18 H 20 N 3 NaO 3 S, molecular weight: 381.43, structural formula: [0003] [0004] Rabeprazole sodium is a benzimidazole compound. It is a second-generation proton pump inhibitor that specifically inhibits parietal cells H + , K + -ATPase system to block the last step of gastric acid secretion. The effect is dose-dependent, and can inhibit both basal gastric acid secretion and gastric acid secretion under stimulation. This product is effective against choline and histamine H 2 The receptor has no antagonistic effect. [0005] The salt formation of rabeprazole sodium, patent literature reports all use rabeprazole and sodium hydroxide aqueous solution reaction, be...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/12
Inventor 陶灵刚
Owner HAINAN MEILAN SMITH KLINE PHARMA
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