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Preparation method of high purity nicotinamide and nicotinic acid

A high-purity, nicotinamide technology, applied in organic chemistry and other directions, can solve the problems of difficult separation of nicotinamide, nicotinic acid and catalyst, and achieve the effects of easy industrial production, less pollution, and easy availability of solvents

Inactive Publication Date: 2015-04-08
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the traditional method of synthesizing nicotinamide, there is always the formation of by-product nicotinic acid, which causes the problem of difficult separation of nicotinamide, nicotinic acid and catalyst, and a large amount of post-treatment is required to obtain high-purity nicotinamide product Work

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 1000ml four-neck flask, add 121g of 3-cyanopyridine and 339.5g of ethanol, and stir for 30min to completely dissolve the 3-cyanopyridine. Then take 7.275g of sodium hydroxide and dissolve it in 145.5g of water to prepare a 5% NaOH solution. While stirring, add the prepared sodium hydroxide solution, then add 24.2gMnO 2 , heated to 95 ° C for 8 hours. After the reaction, filter to remove the catalyst MnO 2 , then heat up to remove the solvent, and filter to obtain nicotinamide. The content of product is 85%, and yield is 82%.

Embodiment 2

[0022] In a 1000ml four-neck flask, add 121g of 3-cyanopyridine and 412g of ethanol, and stir for 30min to completely dissolve the 3-cyanopyridine. Then take 3.83g of sodium hydroxide and dissolve it in 72.8g of water to prepare a 5% NaOH solution. While stirring, add the prepared sodium hydroxide solution, then add 24.2gMnO 2 , heated to 95 ° C for 8 hours. After the reaction, filter to remove the catalyst MnO 2 , then heat up to remove the solvent, and filter to obtain nicotinamide. The content of the product is 95%, and the yield is 90%.

Embodiment 3

[0024] In a 1000ml four-neck flask, add 121g of 3-cyanopyridine and 460.8g of ethanol, and stir for 30min to completely dissolve the 3-cyanopyridine. Then take 1.21g of sodium hydroxide and dissolve it in 24.2g of water to prepare a 5% NaOH solution. While stirring, add the prepared sodium hydroxide solution, then add 24.2gMnO 2 , heated to 95 ° C for 8 hours. After the reaction, filter to remove the catalyst MnO 2 , then heat up to remove the solvent, and filter to obtain nicotinamide. The content of the product is 99.5%, and the yield is 96%.

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Abstract

The invention provides a preparation method of high purity nicotinamide and nicotinic acid. In an ethanol and water system and in the presence of NaOH and MnO2, 3-cyanopyridine hydrolyzes to obtain high content of nicotinamide and nicotinic acid by adjusting the ratio of ethanol and water. When ethanol and water are in the weight ratio of 19:1, 3-cyanopyridine hydrolyzes to obtain is 99.5% of nicotinamide, and the yield is higher than 95%; and when the ethanol and water are in the weight ratio of 1:9, the 3-cyanopyridine hydrolyzes to obtain 99.5% of nicotinic acid, and the yield is more than 95%. The method has the characteristics of mild reaction conditions, high product purity and high yield; and only by adjusting the content of ethanol, high purity nicotinamide and nicotinic acid are obtained. At the same time, the method has less waste and less pollution, and is beneficial for industrialized production.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for preparing high-purity nicotinamide and nicotinic acid. Background technique [0002] Nicotinamide is a B vitamin, its scientific name is pyridine-3-carboxamide (nicotinamide, niacinamide), nicotinamide, referred to as VB3 or NSA, it is one of the components of coenzymes and coenzymes, and participates in various redox reactions in the body , medically used to treat pellagra, stomatitis, glossitis, liver disease and solar dermatitis, etc.; large doses can lower cholesterol and triglycerides, and its physiological effect is similar to that of niacin, but it has better water solubility and no obvious Vasodilator effect. [0003] Niacin belongs to the vitamin B group compound and is an indispensable nutrient in the human body. Niacin can also be used as a drug intermediate to synthesize a variety of important amide and ester derivative drugs; it is also a very important f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/803C07D213/80C07D213/82
CPCC07D213/82C07D213/80C07D213/803
Inventor 顾福海袁晓路刘敏吴灿平
Owner ANHUI COSTAR BIOCHEM CO LTD
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