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Purifying method for rabeprazole

A technology of rabeprazole and its refining method, which is applied in the field of medicinal chemistry, can solve the problems of loss of raw material drug rabeprazole sodium, huge additional costs, and solvents that cannot be used mechanically, and achieve solvent recovery and mechanical application, high product recovery rate, low cost effect

Inactive Publication Date: 2017-12-22
LIVZON GROUP CHANGZHOU KONY PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the crystal structure of the compound is changed, further clinical trial verification is required, which will incur huge additional costs
In addition, the raw material drug rabeprazole sodium is lost in actual production, and the solvent cannot be applied mechanically, which increases the cost and is uneconomical

Method used

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  • Purifying method for rabeprazole
  • Purifying method for rabeprazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 40g purity is 99.5% rabeprazole crude product (peroxide impurity content is 0.3%) drop in the flask that contains 200ml dichloromethane, add 0.8g silica gel in flask, at 5~10 ℃, stirring adsorption 2 Hour. Filtrate with suction, concentrate the filtrate to dryness, recover the solvent and place it, and apply it to the next batch. Add 100ml of isopropyl ether to the concentrated solution, raise the temperature to 35°C, stir for 30 minutes, then lower the temperature to 5°C and stir for 2 hours, filter with suction, and wash the filter cake with an appropriate amount of isopropyl ether. After drying, 37 g of refined rabeprazole was obtained, with a yield of 92.5%, an HPLC purity of 99.92%, and a peroxide impurity content of 0.04%.

Embodiment 2

[0024] The rabeprazole crude product (peroxide impurity content is 0.2%) that 40g purity is 99.7% is dropped in the flask that contains 150ml methanol, adds 2g gac in the flask, stirs and adsorbs at room temperature for 2 hours. Suction filtration, the filtrate was concentrated to dryness, the solvent was recovered and placed, and used for the next batch. Add 120ml of acetonitrile to the concentrated solution, raise the temperature to 35°C, stir to dissolve, then cool down to 5°C and stir for 2 hours, filter with suction, and wash the filter cake with an appropriate amount of acetonitrile. After drying, 36.5 g of fine rabeprazole was obtained, with a yield of 91.25%, an HPLC purity of 99.91%, and a peroxide impurity content of 0.04%.

Embodiment 3

[0026] 40g purity is 99.6% rabeprazole crude product (peroxide impurity content is 0.35%) drop in the flask that contains 160ml ethyl acetate, add 1g neutral alumina in flask, stir and adsorb at room temperature for 2 hours . Suction filtration, the filtrate was concentrated to dryness, the solvent was recovered and placed, and used for the next batch. Add 200ml of methyl tert-butyl ether to the concentrated solution, raise the temperature to 35°C, stir for 10 minutes, then lower the temperature to 15°C and stir for 2 hours, filter with suction, and wash the filter cake with an appropriate amount of methyl tert-butyl ether. After drying, 38 g of fine rabeprazole was obtained, with a yield of 95%, an HPLC purity of 99.95%, and a peroxide impurity content of 0.03%.

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Abstract

The invention relates to a purifying method for rabeprazole, which includes the steps of: 1) dissolving a rabeprazole crude product, which contains more than 0.1% of a rabeprazole peroxide impurity, in a solvent, adding an adsorbent, stirring the solution for 2-3 h, and filtering the solution to remove the adsorbent; 2) concentrating the filtrate to dry, adding a crystallized solvent to the concentrate, heating the liquid to 35-40 DEG C, stirring the liquid for clarification, reducing temperature to 0-10 DEG C, stirring the solution for 2 h, and performing suction filtration to prepare purified rabeprazole, which is more than 99.9% in purity and is less than 0.1% in content of the peroxide impurity. The purifying method is simple, wherein the solvent can be recovered and is low in consumption, so that the method is low in environment pollution and is high in product purity. The method has important practical application significance in industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry and relates to a method for refining rabeprazole. Background technique [0002] Proton pump inhibitors are used to treat acid-related diseases. They have been widely used in clinical practice and have the best curative effect in the past ten years. They have strong acid-suppressing effect, high specificity, and long duration. As a second-generation proton pump inhibitor, rabeprazole sodium has significantly better clinical effects than the first-generation products. Rabeprazole sodium has a faster onset of action, better acid suppression effect, can continue to suppress acid for 24 hours, short breakthrough at night, drug metabolism is less dependent on CYP2C19 enzymes, and is not affected by genetic polymorphisms [0003] The chemical name of rabeprazole sodium is 2-{[4-(3-methoxypropoxy)-3-methylpyridin-2-yl]methylsulfinyl}-1H-benzimidazole sodium. Molecular formula C 18 h 20 N ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 刘可可张之建何健陈敖
Owner LIVZON GROUP CHANGZHOU KONY PHARMA
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