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Preparation method of lipoic acid

A technology of lipoic acid and lipoic acid ethyl ester, applied in directions such as organic chemistry, can solve the problems of affecting the yield and purity of lipoic acid, material waste, complicated reaction process, etc., and achieves the cost saving of raw materials, shortening reaction time and low cost. Effect

Inactive Publication Date: 2021-03-30
NANJING XINBAI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] In the preparation process of lipoic acid, 1,2,3-trithiahexane-4-pentanoic acid ethyl ester will be produced when the intermediate lipoic acid ethyl ester is prepared, and 6,8-dichlorooctanoic acid ethyl ester sulfur will react with sodium sulfide The reaction produces ethyl 1,2,3-trithiane-4-pentanoate, and ethyl 1,2,3-trithiane-4-pentanoate needs to be reduced to ethyl lipoic acid by sodium sulfite. The reaction process It is extremely complicated, and 1,2,3-trithiahexane-4-pentanoic acid ethyl ester can be transformed into each other with ethyl lipoic acid ester, and will produce a 20% of the 1,2,3-trithiane-4-pentanoic acid ethyl ester by-product causes a lot of waste of materials and affects the final yield and purity of lipoic acid

Method used

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  • Preparation method of lipoic acid
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Examples

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Embodiment 1

[0023] (1) Take sodium sulfide in a beaker, add distilled water to the beaker, heat and stir it below 50°C to dissolve it, and make a 3mol / L sodium sulfide solution; add sulfur to the obtained sodium sulfide solution, stir to dissolve it, Make the concentration of sulfur in the sodium sulfide solution be 3.5mol / L to obtain a mixed solution;

[0024] (2) Add 6,8-dichlorooctanoic acid ethyl ester and distilled water successively in photoreactor and be mixed with 3mol / L 6,8-dichlorooctanoic acid ethyl ester solution, then add phase transfer catalyst in solution, stir and heat up to 82-84°C;

[0025] (3) Add the mixed solution obtained in step (1) dropwise to the reaction solution in step (2) within 180min at a volume ratio of 5:3.5, while using a 1000W xenon lamp and using a 680nm cut-off filter to process the reaction solution. Photocatalysis, and stirring the reaction solution at a speed of 200r / min;

[0026] (4) Add sodium sulfite to the photoreactor after the cyclization re...

Embodiment 2

[0029] (1) Take sodium sulfide in a beaker, add distilled water to the beaker, heat and stir it below 50°C to dissolve it, and make a 3mol / L sodium sulfide solution; add sulfur to the obtained sodium sulfide solution, stir to dissolve it, Make the concentration of sulfur in the sodium sulfide solution be 3.5mol / L to obtain a mixed solution;

[0030] (2) Add 6,8-dichlorooctanoic acid ethyl ester and distilled water successively in photoreactor and be mixed with 3mol / L 6,8-dichlorooctanoic acid ethyl ester solution, then add phase transfer catalyst in solution, stir and heat up to 82-84°C;

[0031] (3) Add the mixed solution obtained in step (1) dropwise to the reaction solution in step (2) at a volume ratio of 5:3 within 180 minutes, while using a 1000W xenon lamp and using a 680nm cut-off filter to filter the reaction solution. Photocatalysis, and stirring the reaction solution at a speed of 200r / min;

[0032] (4) Add sodium sulfite to the photoreactor after the cyclization ...

Embodiment 3

[0035] (1) Take sodium sulfide in a beaker, add distilled water to the beaker, heat and stir it below 50°C to dissolve it, and make a 3mol / L sodium sulfide solution; add sulfur to the obtained sodium sulfide solution, stir to dissolve it, Make the concentration of sulfur in the sodium sulfide solution be 3.5mol / L to obtain a mixed solution;

[0036] (2) Add 6,8-dichlorooctanoic acid ethyl ester and distilled water successively in photoreactor and be mixed with 3mol / L 6,8-dichlorooctanoic acid ethyl ester solution, then add phase transfer catalyst in solution, stir and heat up to 82-84°C;

[0037] (3) Add the mixed solution obtained in step (1) dropwise to the reaction solution in step (2) at a volume ratio of 5:4 within 180 minutes, while using a 1000W xenon lamp and using a 680nm cut-off filter to filter the reaction solution. Photocatalysis, and stirring the reaction solution at a speed of 200r / min;

[0038] (4) Add sodium sulfite to the photoreactor after the cyclization ...

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Abstract

The invention belongs to the field of medicine preparation, and particularly relates to a preparation method of lipoic acid. The preparation method comprises the following steps: carrying out cyclization reaction and desulfurization reaction to prepare ethyl lipoate, and carrying out hydrolytic acidification on the ethyl lipoate to obtain lipoic acid. In the cyclization reaction process and the desulfurization reaction process, light with the wavelength being 680 nm or above is used, and the impurity 1, 2, 3-trithiane ethyl-4-valerate generated in the lipoic acid synthesis process is subjectedto auxiliary catalysis to generate ethyl lipoate. According to the preparation method, the yield of the intermediate product ethyl lipoate of lipoic acid can be increased, so that the final yield oflipoic acid is increased, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the field of medicine preparation, and in particular relates to a preparation method of lipoic acid. Background technique [0002] In the preparation process of lipoic acid, 1,2,3-trithiahexane-4-pentanoic acid ethyl ester will be produced when the intermediate lipoic acid ethyl ester is prepared, and 6,8-dichlorooctanoic acid ethyl ester sulfur will react with sodium sulfide The reaction produces ethyl 1,2,3-trithiane-4-pentanoate, and ethyl 1,2,3-trithiane-4-pentanoate needs to be reduced to ethyl lipoic acid by sodium sulfite. The reaction process It is extremely complicated, and 1,2,3-trithiahexane-4-pentanoic acid ethyl ester can be transformed into each other with ethyl lipoic acid ester, and will produce a 20% of the 1,2,3-trithiane-4-pentanoic acid ethyl ester by-product causes a lot of waste of materials and affects the final yield and purity of lipoic acid. Therefore how to promote the conversion of 6,8-dichloroocta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D339/04
CPCC07D339/04
Inventor 于辉沈飞李栋芸潘爱梅窦文轩
Owner NANJING XINBAI PHARMA
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