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Preparation method for high-purity alpha-lipoic acid

A lipoic acid, high-purity technology, applied in the field of preparation of high-purity α-lipoic acid, can solve the problems of cumbersome synthesis steps, low yield, high route cost, etc., and achieve reduced photolysis, easier agglomeration, and improved yield Effect

Inactive Publication Date: 2019-07-12
SUZHOU HEYAN BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the yield of each synthetic route of lipoic acid is low, generally no more than 60%, and most of the routes are extremely expensive, and the synthetic steps are cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A preparation method of high-purity α-lipoic acid, comprising the steps of:

[0016] S1: Synthesis of ethyl lipoic acid: Add ethyl 6,8-dichlorooctanoate, sulfur, and tetrabutylammonium bromide to the water solvent, raise the temperature to 82°C, slowly add sodium sulfide solution, and react for 5 hours; the reaction is over Afterwards, lower the temperature to 65°C, stand still for about 60 minutes, and separate the layers to obtain ethyl lipoic acid;

[0017] S2: Hydrolysis of ethyl lipoic acid: add sodium hydroxide and tetrabutylammonium bromide, stir, heat up to 50°C, keep warm, and after the reaction, suction filter;

[0018] S3: Acidification of sodium lipoic acid: cool the filtrate obtained in S2 to 5°C, then add hydrochloric acid to adjust the pH to 1 and filter to obtain crude lipoic acid;

[0019] S4: Purification of crude lipoic acid: add the crude lipoic acid obtained in S3 into a mixed solvent (cyclohexane: ethyl acetate = 5-15:1 (w:w)), and stir to complet...

Embodiment 2

[0025] A preparation method of high-purity α-lipoic acid, comprising the steps of:

[0026] S1: Synthesis of ethyl lipoic acid: Add ethyl 6,8-dichlorooctanoate, sulfur, and tetrabutylammonium bromide to the water solvent, raise the temperature to 82°C, slowly add sodium sulfide solution, and react for 5 hours; the reaction is over Afterwards, lower the temperature to 65°C, stand still for about 60 minutes, and separate the layers to obtain ethyl lipoic acid;

[0027] S2: Hydrolysis of ethyl lipoic acid: add sodium hydroxide and tetrabutylammonium bromide, stir, heat up to 60°C, keep warm, after the reaction is completed, suction filter;

[0028] S3: Acidification of sodium lipoic acid: cool the filtrate obtained in S2 to 6°C, then add hydrochloric acid to adjust the pH to 1 and filter to obtain crude lipoic acid;

[0029] S4: Purification of crude lipoic acid: add the crude lipoic acid obtained in S3 into a mixed solvent (cyclohexane:ethyl acetate=7:1 (w:w)), stir to dissolve...

Embodiment 3

[0035] A preparation method of high-purity α-lipoic acid, comprising the steps of:

[0036] S1: Synthesis of ethyl lipoic acid: Add ethyl 6,8-dichlorooctanoate, sulfur, and tetrabutylammonium bromide to the water solvent, raise the temperature to 83°C, slowly add sodium sulfide solution, and react for 5 hours; the reaction is over Afterwards, lower the temperature to 65°C, stand still for about 60 minutes, and separate the layers to obtain ethyl lipoic acid;

[0037] S2: Hydrolysis of ethyl lipoic acid: add sodium hydroxide and tetrabutylammonium bromide, stir, heat up to 50°C-80°C, keep warm, after the reaction, suction filter;

[0038] S3: Acidification of sodium lipoic acid: cool the filtrate obtained in S2 to 7.5°C, then add hydrochloric acid to adjust the pH to 1.5 and filter to obtain crude lipoic acid;

[0039] S4: Purification of crude lipoic acid: add the crude lipoic acid obtained in S3 into a mixed solvent (cyclohexane:ethyl acetate=10:1 (w:w)), stir to dissolve th...

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PUM

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Abstract

The invention relates to the technical field of pharmaceutical preparation, and in particular to a preparation method for high-purity alpha-lipoic acid. The method comprises the following steps: step1, synthesis of ethyl lipoate; step 2, hydrolysis of the ethyl lipoate; step 3, acidification of sodium lipoate; and step 4, purification of crude lipoic acid. According to the method provided by theinvention, purity of a cyclization product is controlled under appropriate conditions, and the crude product is purified at a suitably-lower temperature to limit production of by-products during preparation of the crude product, so that the yield is improved, the yield achieves 65% or more, and the purity is 99% or more.

Description

technical field [0001] The invention relates to the technical field of medicine preparation, more specifically, it relates to a preparation method of high-purity alpha-lipoic acid. Background technique [0002] α-lipoic acid (alpha lipoic acid) is an enzyme present in mitochondria, similar to vitamins, which can eliminate free radicals that accelerate aging and cause disease. Alpha-lipoic acid enters the cells after being absorbed by the intestines in the body. It has both fat-soluble and water-soluble properties, so it can pass through the whole body unimpeded, reach any cell site, and provide comprehensive performance for the human body. It is fat-soluble and water-soluble Universal antioxidant. Dr. Lester Packer of the University of California, Berkeley is the world's top authority on α-lipoic acid and antioxidants. Alpha-lipoic acid is used to prevent and even treat certain diseases such as AIDS, diabetes and its complications, nervous system degeneration and liver dys...

Claims

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Application Information

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IPC IPC(8): C07D339/04
CPCC07D339/04
Inventor 夏增华
Owner SUZHOU HEYAN BIOTECH
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