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Method for preparing acipimox

A technology of sodium tungstate and hydrogen peroxide is applied in the field of preparation of acilimus to achieve the effects of improving blood lipid content, convenient operation and reducing risk

Inactive Publication Date: 2014-03-26
NORTH CHINA UNIV OF WATER RESOURCES & ELECTRIC POWER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, 2,5-dimethylpyrazine is widely used as a spice, and its price remains high, which leads to a higher price of 5-methylpyrazine-2-carboxylic acid prepared through a multi-step reaction, so the synthetic route The cost of raw materials in the production of acipimox is high, the synthetic route is long and complicated, and the total yield is low, so it is not suitable for industrial production

Method used

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  • Method for preparing acipimox
  • Method for preparing acipimox

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: a kind of A method for preparing acipimox, the method comprising the following steps:

[0031] Add 2730ml of concentrated sulfuric acid with a mass concentration of 98% into a 10L glass reactor, add 910.0g of 5-methylpyrazine-2,3-dicarboxylic acid under stirring conditions, heat to 60°C, heat the reaction for 1h, then slowly Add 5.5kg of water, 164.9g of sodium tungstate (Na 2 WO 4 2H 2 O), 623.0g of hydrogen peroxide with a mass concentration of 30%, continued heating and stirring for 8h, cooled and crystallized in an ice bath for 4h, filtered the solid with suction, dried at 100°C for 12h, and prepared 708.0g of the product acipimox. The product yield in this reaction was 92%; the HPLC purity was greater than 99% (area normalization method).

Embodiment 2

[0032] Example 2: A method for preparing acipimox, the method comprising the following steps:

[0033] Add 5.5kg of water into a 10L glass reactor, slowly add 27ml of concentrated sulfuric acid with a mass concentration of 98% under stirring conditions, then add 910.0g of 5-methylpyrazine-2,3-dicarboxylic acid, and heat the reaction at 60°C 1h, then add 164.9g sodium tungstate (Na 2 WO 4 2H 2 O), 623.0g of hydrogen peroxide with a mass concentration of 30%, continued heating and stirring for 8h, cooled and crystallized in an ice bath for 4h, filtered the solid with suction, dried at 100°C for 12h, and prepared 693.5g of the product acipimox. The product yield in this reaction is 90%; the HPLC purity is greater than 99% (area normalization method).

Embodiment 3

[0034] Example 3: A method for preparing acipimox, the method comprising the following steps:

[0035] Add 2000ml of concentrated hydrochloric acid with a mass concentration of 36% into a 10L glass reactor, then add 910.0g of 5-methylpyrazine-2,3-dicarboxylic acid, heat at 70°C for 1.5h, then slowly add 5.5kg of water , and then add 82.5g sodium tungstate (Na 2 WO 4 2H 2 O), 680.0g of hydrogen peroxide with a mass concentration of 30%, continued heating and stirring for 10h, cooled and crystallized in an ice bath for 4h, filtered the solid with suction, dried at 100°C for 12h, and prepared 678.1g of the product acipimox. The product yield in this reaction was 88%; the HPLC purity was greater than 98% (area normalization method).

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Abstract

The invention relates to a method for preparing lipid lowering medicament acipimox. Acipimox is prepared by synthetic reaction by using 5-methylpyrazine-2,3-dicarboxylic acid, water, acid, sodium tungstate and hydrogen peroxide as raw materials, wherein a mol ratio of 5-methylpyrazine-2,3-dicarboxylic acid, acid, hydrogen peroxide to sodium tungstate is 1:0.05-5:1-10:0.04-0.2. Acipimox is prepared by the method by one-step reaction, purity of the product exceeds 99.5% through once recrystallization, yield exceeds 80%, and the method is suitable for industrial batch production. The method has advantages of low cost of raw material, short synthetic route, simple technology, convenient operation, simple post-treatment, safety and environmental protection of the solvent, basic no pollution of the oxidizing agent, no need of organic solvent in the reaction process, greening, environmental protection, small pollution and wide market prospect, and the production cost is less than a half of that of the prior method.

Description

technical field [0001] The invention relates to a lipid-lowering drug, in particular to a preparation method of acipimox. Background technique [0002] Acilimus is a niacin derivative used for the treatment of hypercholesterolemia and hypertriglyceridemia, and is a new lipid-lowering drug against lipidation. As the preferred basic lipid-lowering drug, the drug has a good lipid-lowering effect and is widely used in the treatment of hypertriglyceridemia and hypercholesterolemia. Its lipolysis inhibitory activity is 20 times that of niacin. The decomposition of free fatty acids reduces the generation of free fatty acids, which can effectively reduce the risk of coronary heart disease, and the blood lipid content can be improved in a short time after taking the medicine. The dose of this drug is relatively large, but the raw material cost of acipimox remains high. There are few domestic pharmaceutical companies producing the drug, and the price of acipimox is high, which great...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/24
CPCC07D241/24
Inventor 杨光瑞王海荣苗长庆张丽秦德志
Owner NORTH CHINA UNIV OF WATER RESOURCES & ELECTRIC POWER
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