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Preparation method of iguratimod intermediate IV

An intermediate and weight ratio technology, which is applied in the field of medicine and chemical industry, can solve the problems of great harm to the human body, difficulty in mixing, and large environmental pollution, and achieve the effects of improving product purity, facilitating post-processing, and reducing environmental pollution

Inactive Publication Date: 2017-09-15
常州佳德医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new compound was made from nitrone rather than naphtha because it does produce less bad odor when used alone compared to other methods like sulfur dioxide or hydrogen peroxide. Additionally, this new chemical produced an equal amount of pure material but without any unwanted side products that were added during previous steps. Overall, these technical results led to better quality materials being created at large scales.

Problems solved by technology

This patented describes different methods for producing certain substances called intermediates that have various uses within medicine or pharmacy industries. These processes involve reacting specific chemical compounds with ammonia gas at high temperatures under controlled conditions. Existing techniques require expensive reagents like sulfuric acid and formaldehyde, making it challenges to produce these products efficiently without generating unwanted waste materials during manufacturing.

Method used

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  • Preparation method of iguratimod intermediate IV
  • Preparation method of iguratimod intermediate IV
  • Preparation method of iguratimod intermediate IV

Examples

Experimental program
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Effect test

Embodiment 1

[0024] After adding 300mL of nitromethane to the 1000mL reaction flask, add 203g of anhydrous aluminum trichloride in batches, and add 114g of aminoacetonitrile hydrochloride after cooling to room temperature; when the temperature drops below 20℃, add 150g of intermediate III(4 -Phenoxy-3-methanesulfonamido anisole); After stirring for 10 minutes, dry hydrogen chloride gas is introduced, and the reaction is completed by airing for about 15 hours. Slowly add the above reaction solution to 1200g 2mol / L dilute hydrochloric acid, control the temperature below 10℃, stir for 1h after adding, filter, wash the solid with a small amount of water (about 80mL), drain; then use 150mL ethyl acetate Beating, filtering, draining, and drying; then the solid is refluxed with twice the volume of 95% (volume percentage) ethanol for 1 hour to cool, filtered, and the solid is dried until the moisture content is qualified to obtain the final product (α-amino-2-methoxy- 4-Methanesulfonamido-5-phenoxy...

Embodiment 2

[0028] After adding 300mL of nitromethane to the 1000mL reaction flask, add 203g of anhydrous aluminum trichloride in batches, and add 114g of aminoacetonitrile hydrochloride after cooling to room temperature; when the temperature drops below 20℃, add 150g of intermediate III(4 -Phenoxy-3-methanesulfonamido anisole); After stirring for 10 minutes, dry hydrogen chloride gas is introduced, and the reaction is completed by airing for about 15 hours. Slowly add the above reaction solution to 1200g 1mol / L dilute hydrochloric acid, control the temperature below 10℃, stir for 1h after adding, filter, wash the solid with a small amount of water (about 80mL), drain; then use 150mL ethyl acetate Beating, filtering, draining, and drying; then the solid is refluxed with twice the volume of 95% (volume percentage) ethanol for 1 hour to cool, filtered, and the solid is dried until the moisture content is qualified to obtain the final product (α-amino-2-methoxy- 4-Methanesulfonamido-5-phenoxy...

Embodiment 3

[0030] After adding 300mL of nitromethane to the 1000mL reaction flask, add 203g of anhydrous aluminum trichloride in batches, and add 114g of aminoacetonitrile hydrochloride after cooling to room temperature; when the temperature drops below 20℃, add 150g of intermediate III(4 -Phenoxy-3-methanesulfonamido anisole); After stirring for 10 minutes, dry hydrogen chloride gas is introduced, and the reaction is completed by airing for about 15 hours. Slowly add the above reaction solution to 1200g 4mol / L dilute hydrochloric acid, control the temperature below 10℃, stir for 1h after adding, filter, wash the solid with a small amount of water (about 80mL), drain; then use 150mL ethyl acetate Beating, filtering, draining, and drying; then the solid is refluxed with twice the volume of 95% (volume percentage) ethanol for 1 hour to cool, filtered, and the solid is dried until the moisture content is qualified to obtain the final product (α-amino-2-methoxy- 4-Methanesulfonamido-5-phenoxy...

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Abstract

The invention discloses a method for preparing an iguratimod intermediate IV, which belongs to the technical field of medicine and chemical industry. The present invention replaces nitrobenzene with nitromethane as the preparation of Alamod intermediate IV (α-amino-2-methoxy-4-methanesulfonamido-5-phenoxyacetophenone hydrochloride ) solvent, the weight yield of the prepared Alamod intermediate IV can reach 102~105%, and the purity can reach more than 99%; in addition, the present invention adopts nitromethane as the solvent of reaction and also has the following advantages: weak smell , less pollution, less harm to the human body, easy post-processing of the product, improved purity, and no genotoxic impurity nitrobenzene residue in the final product.

Description

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Claims

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Application Information

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Owner 常州佳德医药科技有限公司
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