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Industrial preparation method for riboflavine sodium phosphate

A technology of sodium riboflavin phosphate and riboflavin phosphate, which is applied in the field of industrial preparation of sodium riboflavin phosphate, can solve problems such as failure to meet quality requirements, high activity of phosphorus oxychloride, and poor reaction selectivity. Achieve the effects of easy mastery of production technology, low production cost and mild production conditions

Active Publication Date: 2011-10-05
HUBEI GUANGJI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this preparation method, because the activity of phosphorus oxychloride is too high, it forms a ring with riboflavin 4', the 5'-position hydroxyl and also forms a ring with 3', 5'-position and 3', 4'-position, and its reaction selectivity It is extremely poor and generates many other by-products, and the final product has poor purity and poor quality, and cannot reach the quality requirements of riboflavin sodium phosphate in various pharmacopoeias at home and abroad.

Method used

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  • Industrial preparation method for riboflavine sodium phosphate
  • Industrial preparation method for riboflavine sodium phosphate
  • Industrial preparation method for riboflavine sodium phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) Phosphorylation reaction of riboflavin to generate riboflavin cyclic phosphate;

[0032] Extract 180kg (that is, 4390mol) of acetonitrile into the reaction tank, open the jacket and cool the salt to below 8°C. Open the vacuum valve of the pyridine metering tank to accurately extract 126kg of pyridine (1064mol) into the pyridine metering tank. After evacuating the vacuum, open the bottom valve of the metering tank and slowly add pyridine to the reaction tank. ℃. Then accurately extract 244kg (i.e. 1195mol) of phosphorus oxychloride into the metering tank, slowly drip into the reaction tank, and the temperature of the reaction solution is lower than 5°C. 80kg of acetonitrile (i.e. 1951mol) is sucked into the mixed liquid metering tank earlier, and then 12kg of purified water (i.e. 665mol) is sucked in. Close the vacuum valve, the temperature in the reaction tank drops below 5°C, and slowly add the acetonitrile-water mixture to ensure that the temperature is below 10°...

Embodiment 2

[0041] Take 200kg (that is, 4878mol) of acetonitrile into the reaction tank, open the jacket ice salt and cool down to below 5°C. Take 126kg (i.e. 1615mol) of pyridine into the pyridine metering tank. After evacuating the vacuum, open the bottom valve of the metering tank and slowly add pyridine into the reaction tank. Take 260kg (that is, 1688mol) of phosphorus oxychloride into the metering tank, slowly add it to the reaction tank, and the temperature of the reaction solution is lower than 5°C. First pump 100 g (ie 2439 mol) of acetonitrile in the mixed liquid metering tank, and add 10 kg (ie 555 mol) of purified water. When the temperature in the reaction tank drops below 5°C, start to slowly add the acetonitrile-water mixture to ensure that the temperature of the reaction solution is below 10°C during the process. Add 100kg (ie 266mol) riboflavin and react at 5-10°C for 8h. After suction filtration, soak the riboflavin cyclic phosphate filter cake twice with 100kg of acet...

Embodiment 3

[0050] Take 200kg (that is, 2632mol) tetrahydrofuran into the reaction tank, open the jacket ice salt and cool down to below 5°C. Take 126kg (i.e. 1615mol) of pyridine into the pyridine metering tank. After evacuating the vacuum, open the bottom valve of the metering tank and slowly add pyridine into the reaction tank. Take 260kg (that is, 1688mol) of phosphorus oxychloride into the metering tank, slowly add it to the reaction tank, and the temperature of the reaction solution is lower than 5°C. First pump 80kg (ie 1111mol) tetrahydrofuran into the mixed liquid metering tank, and add 12kg (ie 665mol) purified water. When the temperature in the reaction tank drops below 5°C, start to slowly add the acetonitrile-water mixture to ensure that the temperature of the reaction solution is below 10°C during the process. Add 100kg (ie 266mol) of riboflavin (B2) and react at 5-10°C for 8h. After suction filtration, soak the riboflavin cyclic phosphate filter cake with an appropriate a...

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Abstract

The invention discloses an industrial preparation method for riboflavin sodium phosphate, which uses riboflavin, phosphorus oxychloride, pyridine and purified water as initial raw materials, and comprises the following steps of: 1) carrying out phosphation reaction on riboflavin to generate riboflavin cyclophosphate; 2) hydrolyzing the riboflavin cyclophosphate to generate riboflavin phosphate; 3) carrying out salifying reaction on the riboflavin phosphate to generate riboflavin sodium phosphate; and 4) refining the riboflavin sodium phosphate. The riboflavin sodium phosphate product prepared by the preparation method provided by the invention has high quality and low impurity content, and can reach the quality requirement on riboflavin sodium phosphate in various current pharmacopoeias at home and abroad. The preparation method has the advantages of mild production conditions, no requirements for very low temperature, extra-high temperature and extra-high pressure, no special requirement on equipment, easiness in mastery of production technique, low production cost of a product, high product purity and easiness in recycling of wastes, and is suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation, and specifically refers to an industrial preparation method of riboflavin sodium phosphate. Background technique [0002] Riboflavin (B 2 ) is a component of many enzymes in human metabolism, which can be synthesized by plants, yeasts, fungi and other microorganisms, but cannot be synthesized by animals themselves. The lack of riboflavin in the body mainly manifests as lesions of epidermal tissues, such as angular cheilitis, cheilitis, glossitis, keratitis, and male scrotum. Due to the poor water solubility of riboflavin, its scope of use in medicine is limited to a certain extent. Making it into water-soluble phosphate can expand its scope of use and be used in industries such as medicine, food additives, feed, and veterinary medicine. Clinically, riboflavin sodium phosphate is commonly used to make injections for the treatment of aphtha, skin diseases, vitamin deficiency and othe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6561
Inventor 巨修炼何谧郭韶智郑志长孙先明
Owner HUBEI GUANGJI PHARMA
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