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

Refining method of 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole

A refining method, pyridyl-based technology, applied in the field of medicine and chemical industry, can solve the problems of high impurities in the product, and achieve the effect of high purity, low cost and simple operation

Inactive Publication Date: 2017-12-15
赵剑锋
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the technical problem that the product prepared by the existing topinostat preparation method has more impurities, and to provide a kind of 5-(2-cyano-4-pyridyl)-3-(4-pyridyl) The purification method of -1,2,4-triazole

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 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole
  • Refining method of 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole
  • Refining method of 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A method for refining 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole in this embodiment comprises the following steps:

[0032] The chemical formula of a, 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole is:

[0033]

[0034] b, 1g formula (I) compound crude product is added in 10ml alkaline ethanol, and described alkaline ethanol is the mixed solution of sodium hydroxide and ethanol, and the mass concentration of sodium hydroxide in alkaline ethanol is 10%, reacts Control the temperature of the system to 10°C, stir until it dissolves and then filter, adjust the pH value of the filtrate to 6.5 with hydrochloric acid with a concentration of 6M, then control the temperature of the reaction system to 10°C, stir to fully separate out the solid, filter, and rinse the filter cake with ethanol washed, and air-dried at 80°C to obtain an off-white solid;

[0035] c. Add 0.5 g of the off-white solid obtained in step b into 5ml of DMF, rapidly raise the temperature to 13...

Embodiment 2

[0037] A method for refining 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole in this embodiment comprises the following steps:

[0038] The chemical formula of a, 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole is:

[0039]

[0040] b, 1g formula (I) compound crude product is added in 25ml alkaline ethanol, and described alkaline ethanol is the mixed solution of sodium hydroxide and ethanol, and the mass concentration of sodium hydroxide in alkaline ethanol is 3%, reacts Control the temperature of the system to -20°C, stir until it dissolves and then filter, adjust the pH value of the filtrate to 6.0 with 1M hydrochloric acid, then control the temperature of the reaction system to -10°C, stir to fully separate out the solid, filter, and use as a filter cake Rinse with ethanol, and air-dry at 80°C to obtain off-white solid;

[0041] c. Add 0.5 g of the off-white solid obtained in step b into 0.5ml of DMF, rapidly raise the temperature to 120°C to dissolve the system, ...

Embodiment 3

[0043] A method for refining 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole in this embodiment comprises the following steps:

[0044] The chemical formula of a, 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole is:

[0045]

[0046] b. Add 0.5g of the crude compound of formula (I) into 2.5ml of alkaline ethanol, the alkaline ethanol is a mixture of sodium hydroxide and ethanol, and the mass concentration of sodium hydroxide in the alkaline ethanol is 35%, Control the temperature of the reaction system to 25°C, stir until it dissolves and then filter, adjust the pH value of the filtrate to 7.5 with 3M hydrochloric acid, then control the temperature of the reaction system to 25°C, stir to fully separate the solid, filter, and use as a filter cake Rinse with ethanol, and air-dry at 80°C to obtain off-white solid;

[0047] c. Add 0.2 g of the off-white solid obtained in step b into 3ml of DMF, rapidly raise the temperature to 140°C to dissolve the system, then cool down ...

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 relates to a refining method of 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole, and aims to solve the technical problem that more impurities exist in a product prepared by an existing topiroxostat preparation method. The invention is characterized by adding a 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole crude product into alkaline ethanol; filtering after stirring until realizing dissolved clarification; regulating a pH (Potential of Hydrogen) value of filtrate to 6.0 to 8.0 by using hydrochloric acid; then controlling the temperature of a reaction system to be -10 to 25 DEG C; stirring, and fully separating out solid; carrying out solid-liquid separation; leaching the solid by an organic solvent, and blowing air for drying under 80 DEG C, thus obtaining off-white solid; adding the off-white solid into the organic solvent; rapidly heating, and carrying out dissolved clarification on the system; then cooling to 5 to 25 DEG C; standing and crystallizing; filtering and drying, thus obtaining refined 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a method for refining 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole. Background technique [0002] 5-(2-cyano-4-pyridyl)-3-(4-pyridyl)-1,2,4-triazole is a pharmaceutical raw material that can be used to treat gout, hyperuricemia, etc. Patent CN104151297B discloses the preparation method of the compound, using methylisonicotinic acid-N-oxide as the starting material, in the presence of copper catalyst, metal cyanide and dimethylcarbamoyl chloride, to generate 2-cyanoisonicotinic acid Methyl ester, methyl 2-cyanoisonicotinate is hydrolyzed to 2-cyanoisoniazid, and finally condensed with 4-cyanopyridine to obtain 5-(2-cyano-4-pyridyl)-3-( 4-pyridyl)-1,2,4-triazole, i.e. topicrestat, the reaction formula is as follows: [0003] [0004] But the product obtained by this preparation method has more impurities, and the purity is only 98.5%. At present, there is no...

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): C07D401/14
CPCC07D401/14
Inventor 赵剑锋
Owner 赵剑锋
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