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Preparation method of cocarboxylase tetrahydrate

A technology of tetrahydrate cocarboxylase and dehydrating agent, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, and organic chemistry, etc.

Active Publication Date: 2010-07-28
西藏中卫诚康药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the actual operation process, it was found that the method was not practical, and the reaction could hardly be carried out normally.

Method used

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  • Preparation method of cocarboxylase tetrahydrate

Examples

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Comparison scheme
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Embodiment 1

[0031] Add 60g of pyrophosphoric acid into the reactor, stir at 100°C for 1 hour, add 20g of vitamin B1, and then heat to 120°C for 30 minutes to dissolve the solid completely, add 20g of phosphorus pentoxide, and stir until the raw material point completely disappears as detected by TLC (Developer: methanol: water: acetic acid = 2:1:0.5), add water and ethanol solution to precipitate a large amount of off-white solid, filter. Detected cocarboxylase and vitamin B 1 Monophosphates, Vitamin B 1 A mixture of triphosphates, take the solid mixture or dissolve it in 50ml purified water and repeat the above operation once, dissolve the solid in 100ml purified water, extract twice with 2×100ml 70% trioctylamine methyl isobutyl carbinol solution, take the aqueous solution , into a 100ml weakly basic anion exchange resin (D301) column, eluted with purified water, directly introduce the eluate into 1000ml of strongly acidic cation exchange resin (732), elute with purified water, and det...

Embodiment 2

[0034] Add 90g of pyrophosphoric acid into the reactor, stir well at 100°C for 1 hour, add 20g of vitamin B 1 , heated to 120°C and reacted for 30 minutes, added 40g of phosphorus pentoxide, stirred until the TLC detection of the raw material point completely disappeared, cooled, added dropwise purified water to form a transparent solution, added water and ethanol solution to precipitate a large amount of off-white solid, filtered, Take the solid, dissolve the obtained solid in purified water, extract twice with 50% trioctylamine isopropyl ether solution, take the aqueous solution and load it into a weakly basic anion exchange resin (D301) column, elute with purified water, and directly introduce the eluent into In the strongly acidic cation exchange resin (732), elute with purified water, start to receive the eluent when the ultraviolet detection eluent shows fluorescence, and stop receiving the eluent until the ultraviolet detection eluent has no fluorescence, and the eluent ...

Embodiment 3

[0036] Add 70g of pyrophosphoric acid into the reactor, stir well at 130°C for 1 hour, add 20g of vitamin B 1 , then heated to 140°C to react for 30 minutes, added 30 g of phosphorus oxychloride, stirred and reacted until the raw material point detected by TLC disappeared completely, cooled, added purified water dropwise to form a transparent solution, added water and ethanol solution to precipitate a large amount of off-white solid, Filtrate, take the solid, dissolve the obtained solid in purified water, extract twice with trioctylamine solution, take the aqueous solution and put it into a weakly basic anion exchange resin (D301) column, elute with purified water, and directly introduce the eluent into a strongly acidic cation In the exchange resin (732), the purified water is eluted, and the eluent is received when the ultraviolet detection eluent shows fluorescence, and the eluent is received until the ultraviolet detection eluent has no fluorescence, and the eluent is conce...

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Abstract

The invention relates to a preparation method of cocarboxylase tetrahydrate, which is mainly characterized in that pyrophosphoric acid and dehydrating agent are reacted with vitamin B1 under the heating condition to obtain the cocarboxylase tetrahydrate. The method has the advantages that the product yield is improved, the production cost is reduced, the product quality is improved, the environmental pollution is reduced, and the like.

Description

technical field [0001] The invention relates to a preparation method of tetrahydrate cocarboxylase. Background technique [0002] Cocarboxylase Tetrahydrate is a vitamin drug, also known as thiamine tetrahydrate pyrophosphate, which participates in the oxidative decarboxylation of pyruvate and a-ketoglutaric acid in the carbohydrate metabolism in vivo, and is necessary for carbohydrate metabolism , when it is lacking, the oxidation is blocked to form pyruvate, and lactic acid accumulates, which affects the energy supply of the body. The symptoms are mainly manifested in the nervous system, cardiovascular system and digestive system. Clinically, it is commonly used in the treatment of beriberi or Wernicke encephalopathy. It can also be used as an adjuvant therapy for peripheral neuritis and indigestion caused by cocarboxylase tetrahydrate deficiency. Cocarboxylase tetrahydrate chemical name is 4-methyl-3-[(2-methyl-4-amino-5-pyrimidinyl)methyl]-5-(2-pyrophosphoryloxyethyl)t...

Claims

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Application Information

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IPC IPC(8): C07F9/6558
Inventor 曹志华胡军刘烽常迪张勇
Owner 西藏中卫诚康药业有限公司
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