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Resin deamination method in R-lipoic acid synthesis process

A synthesis process, a technology of lipoic acid, applied in the directions of organic chemistry methods, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as yield decline, product deterioration, etc., and achieve simple and mild methods, easy operation, and mild reaction conditions. Effect

Pending Publication Date: 2022-03-15
TECHNO (FUJIAN) FOOD INGREDIENTS CO LTD
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

However, in the subsequent acidification process, the use of hydrochloric acid acidification will cause the product to deteriorate under strong acid conditions, resulting in a decrease in yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The resin deamination method of a kind of R-lipoic acid synthesis process of the present embodiment, its steps are as follows:

[0027] (1) Dissolve 100 g of vortex lipoic acid in 200 g of toluene, add 30 g of R-phenethylamine, stir and crystallize at 3° C. for 2 h, and obtain 72 g of R-phenethylamine lipoic acid double salt through suction filtration;

[0028] (2) the above-mentioned R-phenylethylamine lipoic acid double salt is dissolved in 230g methanol, and the methanol solution containing double salt is obtained after stirring and dissolving for 0.5h; After the pH is greater than 5, pass the above-mentioned methanol solution containing double salt through the column for cation exchange resin adsorption, the flow rate is controlled at 2 times the column volume / h, then add 50ml methanol to elute again, and after the solution is filtered, 400ml R-lipoic acid solution is obtained ;

[0029] (3) After the above-mentioned R-lipoic acid solution was evaporated to dryness...

Embodiment 2

[0033] The resin deamination method of a kind of R-lipoic acid synthesis process of the present embodiment, its steps are as follows:

[0034] (1) Dissolve 100 g of vortex lipoic acid in 200 g of tert-butyl methyl ether, add 40 g of R-phenethylamine, stir and crystallize at 3° C. for 2 hours, and obtain 76 g of R-phenethylamine lipoic acid double salt through suction filtration;

[0035] (2) the above-mentioned R-phenylethylamine lipoic acid double salt is dissolved in 300g ethanol, and the ethanol solution containing double salt is obtained after stirring and dissolving for 0.5h; After the pH is greater than 5, pass the above-mentioned ethanol solution containing double salt through the column for cation exchange resin adsorption, the flow rate is controlled at 2 times the column volume / h, then add 50ml ethanol to elute again, and after the solution is filtered, 450ml R-lipoic acid solution is obtained ;

[0036] (3) After the above-mentioned R-lipoic acid solution was evapo...

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Abstract

The invention discloses a resin deamination method in an R-lipoic acid synthesis process, which comprises the following steps of: performing ion exchange on R-phenylethylamine in R-phenylethylamine lipoic acid double salt by using cation acidic resin to obtain an R-lipoic acid solution, crystallizing and separating to obtain high-purity R-lipoic acid. The problem of deterioration caused by hydrochloric acid acidification is reduced, and the product purity and yield are high. The process method is simple and mild, the resin can be repeatedly used after being treated, the R-phenylethylamine can be obtained after the eluent is subjected to alkali reaction and dehydration, and the R-phenylethylamine can be repeatedly used, so that the production cost is reduced, good economic value is achieved, and a new way is provided for industrial production of the R-lipoic acid.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a resin deamination method in the synthesis process of R-lipoic acid. Background technique [0002] Lipoic acid (R-(+)-alpha lipoic acid) is a coenzyme naturally produced by the human body. It participates in aerobic metabolism to generate energy. It is also a powerful antioxidant. Its antioxidant capacity is 200 times that of vitamin C. It has both fat-soluble and water-soluble properties, and is widely used in the prevention and treatment of heart disease, diabetes and senile dementia. Lipoic acid has the following effects: [0003] (1) Strong anti-oxidation, has the ability to eliminate accelerated aging and disease-causing free radicals; [0004] (2) Stabilize the blood sugar level, which can improve the symptoms of peripheral neuropathy related to diabetes; [0005] (3) Treatment of chronic hepatitis and other liver diseases. [0006] (4) Studies have found th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D339/04C07C209/74C07C209/84C07C211/27
CPCC07D339/04C07C209/74C07C209/84C07B2200/07C07C211/27
Inventor 钟锋刘玲玲李恒李忠毅周健
Owner TECHNO (FUJIAN) FOOD INGREDIENTS CO LTD
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