Method for preparing alpha-lipoic acid

A lipoic acid and sodium lipoic acid technology, applied in the direction of organic chemistry, can solve the problems of difficult to increase yield, cumbersome synthesis steps, and harsh conditions, and achieve the effects of improving purity, reducing the formation of impurities, and being easy to operate

Active Publication Date: 2013-04-24
SHANDONG QIDU PHARMA
View PDF3 Cites 15 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the 1960s, this research reached a certain stage, and several routes that could be industrialized were obtained, but it was difficult to increase the yield
The raw material cost of this method is low, but the yield is only 45%, the yield is low, and the condi

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing alpha-lipoic acid
  • Method for preparing alpha-lipoic acid
  • Method for preparing alpha-lipoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Add 80 g of purified water into a 500 mL beaker, add 21.8 g of sodium sulfide under stirring, dissolve at 35° C., and prepare a sodium sulfide solution.

[0046] Into a 500 mL round bottom flask, 50 g of ethyl 6.8-dichlorooctanoate, 150 g of purified water, 8 g of sulfur, and 3.5 g of tetrabutylammonium bromide were added. Heat to 82°C under stirring, add sodium sulfide solution dropwise, and finish dropping in 1 hour, and the dropping temperature is kept at 70°C. After the dropwise addition, the reaction was continued for 5 hours, the temperature was lowered to 65° C., and the mixture was left to stand for about 60 minutes, and the layers were separated to obtain 48.3 g of ethyl lipoic acid. Then put ethyl lipoic acid, 1600g of drinking water, 24.2g of sodium hydroxide and 1.93g of tetrabutylammonium bromide into the hydrolysis kettle into a 3000mL reaction kettle, stir, heat to 70°C, keep it warm for 13 hours, and pump it out while it is hot. Filter it into a 5L reac...

Embodiment 2

[0050] Add 120g of purified water into a 500mL beaker, add 31.2g of sodium sulfide under stirring, dissolve at 40°C, and prepare a sodium sulfide solution.

[0051] In a 500 mL round bottom flask, 50 g of ethyl 6.8-dichlorooctanoate, 150 g of drinking water, 15 g of sulfur, and 3.5 g of tetrabutylammonium bromide were added. Heat to 84°C under stirring, add sodium sulfide solution dropwise, and finish dropping in 1.5 hours, and keep the dropping temperature at 86°C. After the dropwise addition, the reaction was continued for 5 hours, the temperature was lowered to 65° C., and the mixture was left to stand for about 60 minutes, and the layers were separated to obtain 48.1 g of ethyl lipoic acid. Then put ethyl lipoic acid, 1600g of drinking water, 48.1g of sodium hydroxide and 1.92g of tetrabutylammonium bromide into the hydrolysis kettle into a 3000mL reaction kettle, stir, heat to 50°C, keep it warm for 13 hours, and pump it out while it is hot. Filter into a 5L reaction ket...

Embodiment 3

[0055] Add 100 g of purified water into a 500 mL beaker, add 25 g of sodium sulfide under stirring, dissolve at 37°C, and prepare a sodium sulfide solution.

[0056] In a 500 mL round bottom flask, add 50 g of ethyl 6.8-dichlorooctanoate, 150 g of drinking water, 10 g of sulfur, and 3.5 g of tetrabutylammonium bromide. Heat to 83°C under stirring, add sodium sulfide solution dropwise, and finish dropping in 1.2 hours, the dropping temperature is kept at 84°C. After the dropwise addition, the reaction was continued for 5 hours, the temperature was lowered to 65° C., and the mixture was left to stand for about 60 minutes, and the layers were separated to obtain 47.7 g of ethyl lipoic acid. Then put ethyl lipoic acid, 1600g of drinking water, 54.8g of sodium hydroxide and 1.9g of tetrabutylammonium bromide into the hydrolysis kettle into a 3000mL reaction kettle, start stirring, heat to 80°C, and keep it warm for 13 hours. Suction filter into a 5L reaction kettle, add dropwise 5...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method for preparing alpha-lipoic acid, comprising the following steps: preparing the sodium sulphide liquor, synthesizing lipoic acid ethyl ester, hydrolyzing the lipoic acid ethyl ester, acidizing the sodium thioctate, and purifying the crude product of the lipoic acid. The liquor adopted by the method during the preparation process has no pollution for human bodies, is safe and easy to operate, and has the performances of high lipoic acid purity, high reaction yield and gentle reaction conditions, so that the method is suitable for industrial production on large scales.

Description

Technical field [0001] The present invention involves a method of preparation of α-sulfuric acid, which is a pharmaceutical preparation technology field. Background technique [0002] The chemical name of α-sulfuric acid is (±) -5- [3 ’-(1’ (1 ’, 2’-di-sulfurized cycle pentalate)-] pent acid, and the structure is as shown below: Essence [0003] Alpha Lipoic Acid is an enzyme existence in mitochondria, similar to vitamins, which can eliminate free radicals that accelerate aging and pathogenic.α-sulfuric acid enters the cells through the intestine and enters the cells, which has the characteristics of fat-soluble and water-soluble. Therefore, it can be unobstructed throughout the body.Universal antioxidant.Dr. Packer, Dr. Packer of Berkeley, University of California, is the world's top α-sulfenic acid and antioxidant authority.α-sulfuric acid is used to prevent or even treat certain diseases such as: AIDS, diabetes and its complications, neurological degeneration and liver dysfun...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07D339/04
Inventor 李洁朱建益郑亮刘明明宋彩香于长安张涛
Owner SHANDONG QIDU PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap