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Method for preparing fursultiamine

A technology of furathiamine and tetrahydrofuryl methyl sodium thiosulfate, which is applied in the field of preparation of furathiamine, can solve the problems of abnormal production and high cost, and achieve the effects of reduced production cost, low cost, and reduced production cost

Pending Publication Date: 2019-03-22
HUAZHONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of furathiamine obtained is above 83%, and the product quality meets the standard, which solves the long-term problem of high cost that has plagued the production of furathiamine and cannot be produced normally

Method used

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  • Method for preparing fursultiamine
  • Method for preparing fursultiamine

Examples

Experimental program
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Effect test

Embodiment 1

[0019] In a 500ml three-necked flask with stirring, add 100g of thiothiamine (pure) and 150g of pure water, stir to cool down, and when the temperature drops to 15°C, slowly add 114.72g of hydrogen peroxide aqueous solution with a mass percentage concentration of 25%. , control the reaction temperature to 15℃-30℃, add dropwise for 5 hours, keep the temperature for 0.5h after the reaction, add 5g of activated carbon, decolorize for 1h, filter, filter out the activated carbon, put the obtained filtrate into a 1000 ml three-necked flask with stirring , stirring to cool down, controlling 20 ℃-30 ℃, adding 80g 25% sodium hydroxide aqueous solution dropwise, adjusting the pH of the solution system to 11-12, the dropping time was 2 hours, the dropwise addition was completed, the temperature was kept stirring for 0.5 hours, and then 80 g tetrahydrofuran methyl group was added. Sodium thiosulfate, controlled at 20°C-30°C, kept stirring for 4 hours, filtered to obtain the crude furanthia...

Embodiment 2

[0021] In a 500ml three-necked flask with stirring, add 100g of thiothiamine (pure) and 150g of pure water, stir to cool down, and when the temperature drops to 15°C, add 95.60g of hydrogen peroxide aqueous solution with a concentration of 30% by mass dropwise , control the reaction temperature to 15℃-30℃, add dropwise for 4 hours, keep the temperature for 0.5h after the reaction, add 5g activated carbon, decolorize for 1h, filter, filter out the activated carbon, put the obtained filtrate into a 1000 ml three-necked flask with stirring , stirring and cooling, controlling 20 ℃-30 ℃, adding 112g 25% potassium hydroxide aqueous solution dropwise, adjusting the pH of the solution system to 11-12, the dropping time was 2 hours, the dropping was completed, and the temperature was kept stirring for 0.5 hours, and then 80g tetrahydrofuran methyl sulfide was added. Substitute sodium sulfate at 20°C-30°C, keep stirring for 4 hours, filter to obtain the crude furanthiamine, recrystallize...

Embodiment 3

[0023] In a 500ml three-necked flask with stirring, add 100g of thiothiamine (pure) and 150g of pure water, stir to cool down, and when the temperature drops to 15°C, dropwise add 104.30g of an aqueous hydrogen peroxide solution with a concentration of 27.5% by mass, Control the reaction temperature to 15℃-30℃, add the reaction dropwise for 6 hours, keep the temperature for 0.5h after the reaction, add 5g of activated carbon, decolorize for 1h, filter, filter out the activated carbon, put the obtained filtrate into a 1000 ml three-necked flask with stirring, Stir and cool down, control 20℃-30℃, add 67g of 30% sodium hydroxide aqueous solution dropwise, adjust the pH of the solution system to 11-12, add dropwise for 2 hours, end the dropwise addition, keep stirring for 1 hour, then add 80g of tetrahydrofuran methylthio Sodium sulfate, controlled at 20°C-30°C, kept stirring for 4 hours, filtered to obtain the crude furanthiamine, recrystallized with water, filtered, and dried to ...

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Abstract

The invention relates to a method for preparing fursultiamine. By adopting the method, fursultiamine is prepared from sulfuric acid thiamine as a main raw material for replacing a conventional process. According to the conventional process, cycle opening and condensation of sulfuric acid thiamine are implemented, the cost is high, and the steps are complex. By adopting the method, cycle opening ofthe sulfuric acid thiamine obtained after oxidation is implemented under an alkali condition, and the sulfuric acid thiamine is condensed with tetrahydrofuran methyl sodium thiosulfate to generate fursultiamine. Steps are simplified, the energy consumption is reduced, and the cost is greatly reduced. Massive application of nitrate in the thiamine mononitrate preparation process and application ofstrong acid gas hydrochloric acid and organic solvents in the thiamine hydrochloride preparation process are avoided, so that the method is green and environmental-friendly, and environment pollutionand potential safety hazard are eliminated. The yield of the fursultiamine is increased to 83% or greater, the product quality meets standards, the difficulty of high cost which obstructs fursultiamine production for a long time can be solved, and the method is a simple and feasible clean and environmental-friendly process route.

Description

technical field [0001] The present invention relates to a preparation method of furanthiamine. Background technique [0002] Fursthiamine is a derivative of vitamin B1, also known as long-acting vitamin B1. It is suitable for the treatment of beriberi or Wernicke encephalopathy due to vitamin B1 deficiency. It can also be used for the adjuvant treatment of peripheral neuritis and indigestion caused by vitamin B1 deficiency. [0003] At present, the synthesis process of furanthiamine at home and abroad is formed by the condensation of thiamine hydrochloride after ring-opening, and the preparation of thiamine hydrochloride is from the oxidation of thiamine hydrochloride to thiamine sulfate, adding nitrate and converting it into thiamine nitrate, and then passing through hydrochloric acid. The conversion into thiamine hydrochloride is expensive, and the steps are lengthy, and hydrochloric acid gas must be prepared during the conversion, and flammable and explosive organic solve...

Claims

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Application Information

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IPC IPC(8): C07D405/12C07D415/00
CPCC07D405/12C07D415/00
Inventor 王勇付林魏旭力李桂莲曾建华
Owner HUAZHONG PHARMA
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