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Preparation method of niacin

A technology of nicotinic acid and concentrated sulfuric acid, applied in organic chemistry and other directions, can solve the problems of difficult industrial production, low yield, environmental pollution, etc., and achieve the effects of easy operation, easy reaction process and wide market sources.

Inactive Publication Date: 2019-04-19
安徽泰格生物技术股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has certain pollution to the environment
[0009] 4. Electrooxidation method: This method is carried out at room temperature, and 3-picoline is electrolyzed in the electrolytic cell of the ion exchange membrane. This method is in the laboratory stage, and there are certain conditions for large-scale production, and the yield is not high
Not easy to industrialize

Method used

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  • Preparation method of niacin

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Embodiment 1

[0033] This embodiment relates to a preparation method of niacin, comprising the following steps:

[0034] 1) In a there-necked flask with 2000ml of condenser tube, under mechanical stirring, add 160 grams of aniline, 192 grams of nitrobenzene, 320 grams of copper sulfate, 640 grams of glycerin, slowly add 160 grams of 98% concentrated sulfuric acid dropwise, the temperature Control at 20°C, add concentrated sulfuric acid dropwise, add 400ml of deionized water dropwise, add 10 grams of catalyst sodium chlorate, control the temperature at 95°C, keep warm for 6 hours, after cooling down to room temperature, filter, filter cake Wash with water until neutral, dry under reduced pressure at 50°C for 4-6 hours to obtain copper quinoline;

[0035] 2) Add the dried copper quinoline into a 1000ml three-neck flask, add 40ml of 10%-20% sodium hydroxide solution under mechanical stirring, adjust the pH to 8-9, heat up to 90°C, and keep warm for 3 hours. Alkaline hydrolysis is completed, l...

Embodiment 2

[0039] The operation was the same as that in Example 1, and the catalyst sodium chlorate was added to 15 grams, and the obtained nicotinic acid product had a purity of 99.7% and a yield of 84%.

Embodiment 3

[0041] The operation is the same as in Example 1, and the catalyst sodium chlorate is added to 20 grams, and the obtained nicotinic acid product has a purity of 99.7% and a yield of 85%.

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Abstract

The invention belongs to the field of organic compound synthesis, and particularly relates to a preparation method of niacin. The method comprises the following steps that 1, aniline, nitrobenzene, copper sulfate, glycerinum and concentrated sulfuric acid are adopted as raw materials, and under the catalytic effect of sodium chlorate, a reaction is performed to obtain copper 8-hydroxyquinolinate;2, the copper 8-hydroxyquinolinate is sequentially subjected to alkaline hydrolysis and acid treatment to obtain 2,3-pyridinedicarboxylic acid, and decarboxylation is performed to prepare niacin. Themethod has the advantages of being low in raw material cost, small in investment, low in product cost, stable in quality and the like, operation is easy, and waste is little, and discharge and testament of waste gas, water and industrial residues can be reduced. The purity of the crude niacin obtained through the method can reach up to 95% or above, and the refined purity is 99.7%; the product yield can reach up to 85%.

Description

technical field [0001] The invention relates to the field of organic compound synthesis, in particular to a preparation method of nicotinic acid. Background technique [0002] Niacin also known as vitamin B 3 Or vitamin PP, its structural formula is: [0003] [0004] Molecular formula: C 6 h 5 NO 2 , molecular weight 123.11, appearance is white or off-white powder, easily soluble in alkali solution, soluble in boiling water or ethanol, slightly soluble in cold water, stable in dry state. Heat resistant, able to sublime. Nicotinic acid is also known as nicotinic acid and anti-peaceae factor. In the human body also includes its derivative nicotinamide or nicotinamide. It is one of the 13 kinds of vitamins necessary for the human body. It is a water-soluble vitamin and belongs to the vitamin B group. Nicotinic acid is converted into nicotinamide in the human body. Niacinamide is a component of coenzyme Ⅰ and coenzyme Ⅱ. It participates in lipid metabolism in the bod...

Claims

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Application Information

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IPC IPC(8): C07D213/803
CPCC07D213/803
Inventor 伏传久陈修陈斌魏升平朱东来
Owner 安徽泰格生物技术股份有限公司