Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Refining method of omeprazole

A technology of omeprazole and a purification method is applied in the field of purification of 5-methoxy-2-[[methyl]sulfinyl]-1H-benzimidazole, and can solve the problem of low dispersibility of omeprazole , unsuitable for industrial production, large amount of impurities in omeprazole, etc., to reduce the risk of increased impurities, facilitate pH adjustment, and improve the effect of refining

Pending Publication Date: 2021-01-08
JIANGSU ZHONGBANG PHARMA +1
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the first two articles adopted the acidification after the crude product of omeprazole was salted, and CN1160050A adopted the acidification of solid acid salt in aqueous solution, and the finally obtained omeprazole was low in content due to containing a large amount of inorganic salts, and due to the final Omeprazole is precipitated in the water solvent. Omeprazole has low dispersion and high viscosity, which is difficult to filter or centrifuge, and is not suitable for industrial production; CN104592201 uses carbon dioxide for acidification. Since omeprazole is more sensitive to pH, the flow of carbon dioxide is controlled. If it is not good, it will easily make omeprazole produce a lot of impurities, and the use of carbon dioxide gas is not suitable for industrial production
The final refined solvent of the above two patents is water, and omeprazole has poor stability in aqueous solution and is easy to produce impurities in the post-treatment process; what CN109206406 adopted is a supercritical fluid chromatography system, which is only suitable for a small amount of research and is not suitable for Suitable for industrial production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Refining method of omeprazole
  • Refining method of omeprazole
  • Refining method of omeprazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Omeprazole refining process:

[0038] Step 1: Pump 5.0kg of purified water into a 20L reaction kettle, then put 2.0kg of sodium hydroxide into the kettle, and stir at room temperature until it dissolves. Drop into omeprazole crude product 1.0kg (HPLC:98.5%, as figure 1 ), stirred at room temperature until dissolved. Pump 2.5kg of dichloromethane into the kettle, stir at room temperature for 15±5 minutes, let stand and separate the liquid, the dichloromethane phase enters the waste water bucket, and the upper water layer is added to the clean reaction kettle. Add 30g of EDTA and 36g of sodium dithionite to the water layer.

[0039] Step 2: Pump 5 kg of dichloromethane into the water phase kettle, and adjust the pH to 8.5 with sodium bicarbonate. After pH adjustment, let stand and separate liquids. The aqueous phase was extracted with 2 kg of dichloromethane. The upper aqueous phase enters the waste water tank, and the organic phase is combined and pumped into a clea...

Embodiment 2

[0042] Step 1: Pump 6.0kg of purified water into a 20L reaction kettle, then put 2.7kg of sodium carbonate into the kettle, and stir at room temperature until it dissolves. Drop into omeprazole crude product 1.0kg (HPLC:98.5%, as figure 1 ), stirred at room temperature until dissolved. Pump 3kg of ethyl acetate into the kettle, stir at room temperature for 15±5 minutes, let it stand and separate the liquid, the ethyl acetate phase enters the waste water bucket, and the upper water layer is added to the clean reaction kettle. Add 30g of EDTA and 18g of sodium dithionite to the water layer.

[0043] Step 2: Pump 5 kg of dichloromethane into the water phase kettle, and adjust the pH to 7.0 with glacial acetic acid. After pH adjustment, let stand and separate liquids. The aqueous phase was extracted with 2 kg of dichloromethane. The upper aqueous phase enters the waste water tank, and the organic phase is combined and pumped into a clean reactor.

[0044] Step 3: Control the ...

Embodiment 3

[0046]Step 1: Pump 5.0kg of purified water into a 20L reaction kettle, then put 2.8kg of potassium hydroxide into the kettle, stir at room temperature until dissolved. Drop into omeprazole crude product 1.0kg (HPLC:98.5%, as figure 1 ), stirred at room temperature until dissolved. Pump 3kg of toluene into the kettle, stir at room temperature for 15±5 minutes, let stand and separate the liquid, the toluene phase enters the waste water bucket, and the upper water layer is added to the clean reaction kettle. 15g of EDTA, 17g of tetrasodium ethylenediaminetetraacetic acid, and 72g of sodium dithionite were added to the water layer.

[0047] Step 2: Pump 5 kg of dichloromethane into the water phase kettle, and adjust the pH to 7.5 with glacial acetic acid. After pH adjustment, let stand and separate liquids. The aqueous phase was extracted with 2 kg of dichloromethane. The upper aqueous phase enters the waste water tank, and the organic phase is combined and pumped into a clean...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a refining method of omeprazole, and belongs to the field of chemical synthesis. The method comprises the following steps: dissolving, decolorizing, washing, pH value regulating, extracting and filtering to obtain the omeprazole fine product. According to the invention, the refining effect is good, the purity can reach 99.8% or above, the yield is 90% or above, and the method has the advantages of being easy to operate, low in uncontrollability and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, specifically a method for refining omeprazole, more precisely 5-methoxy-2-[[(4-methoxy-3,5-dimethyl-2-pyridyl ) The refining method of methyl]sulfinyl]-1H-benzimidazole. Background technique [0002] Omeprazole is the first-generation benzimidazole gastric acid proton pump inhibitor developed by Astra Company in Sweden. It has a strong inhibitory effect on gastric acid, and its curative effect is better than that of H 2 receptor antagonists and prostaglandin E 2 , sucralfate, colloidal bismuth and high-dose antacids can quickly improve the symptoms of peptic ulcer and reflux esophagitis. It is mainly used clinically for gastric ulcer and duodenal ulcer. Omeprazole combined with antibiotics in combination with dual and triple drug regimens can be used to treat peptic ulcers associated with Helicobacter pylori (HP); for reflux esophagitis, gastrinoma (Zollinger-Ellison syndrome) ; Omeprazole ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 李维思黄双薛谊杨晓波张晓晴
Owner JIANGSU ZHONGBANG PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com