Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of preparation method of diammonium glycyrrhizinate

A technology of diammonium glycyrrhizinate and ammonium chloride is applied in the directions of steroids, organic chemistry, etc., can solve the problems of n-butanol solvent residue, long synthesis steps, low product content, etc., and achieves convenient operation procedures and good color. , high yield and high content

Active Publication Date: 2018-09-14
JIANGSU TIANSHENG PHARMA
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis method of diammonium glycyrrhizinate is generally to use solvent to extract glycyrrhizic acid from licorice and then synthesize it. This method has long synthesis steps, high cost, and needs to use a large amount of solvent. The used solvent is not conducive to environmental protection, and The resulting product contains less
[0004] In addition, there are bibliographical reports to use monoammonium glycyrrhizinate as raw material to synthesize diammonium glycyrrhizinate, but there are disadvantages of extracting active ingredients with n-butanol, high loss rate, low yield, and residual n-butanol solvent

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 300g of monoammonium glycyrrhizinate and 1500ml of 25% sodium hydroxide solution were heated to 90°C and refluxed for 12 hours, and after the temperature was lowered to 0°C, the pH value was adjusted to 1-2 with 40% hydrochloric acid solution; White solid; wash twice with hydrochloric acid aqueous solution with a pH value of 1-2, then dissolve the white solid in absolute ethanol, add ammonia water and ammonium chloride until the pH is 7-8, and obtain the crude product of diammonium glycyrrhizinate. Add the crude product of diammonium glycyrrhizinate into 85% acetic acid, and heat to reflux. After the solution is clear, add activated carbon for decolorization, filter, and the filtrate is still for crystallization. Gained crystals were recrystallized through 80% ethanol according to the previous method to obtain diammonium glycyrrhizinate elaboration (content 98.5%, 99.4%) with better quality.

Embodiment 2

[0025] Heat 300g of monoammonium glycyrrhizinate and 1500ml of 30% sodium hydroxide solution to 90°C and reflux for 12 hours, then adjust the pH value to 1-2 with 30% hydrochloric acid solution after cooling down to 0°C; keep warm for 1 hour and filter to obtain white Solid; wash twice with hydrochloric acid aqueous solution with a pH value of 1-2, then dissolve the white solid in absolute ethanol, add ammonia water and ammonium chloride until the pH is 7-8, and obtain the crude product of diammonium glycyrrhizinate. Add the crude product of diammonium glycyrrhizinate into 80% acetic acid, and heat to reflux. After the solution is clear, add activated carbon for decolorization, filter, and the filtrate is still for crystallization. Then the obtained crystals were recrystallized through 75% ethanol according to the previous method to obtain diammonium glycyrrhizinate elaboration (content 98.5%, 99.4%) with better quality.

Embodiment 3

[0027] Heat 300g of monoammonium glycyrrhizinate and 1500ml of 30% sodium hydroxide solution to 90°C and reflux for 12 hours, then adjust the pH value to 1-2 with 30% hydrochloric acid solution after cooling down to 0°C; keep warm for 1 hour and filter to obtain white Solid; wash twice with hydrochloric acid aqueous solution with a pH value of 1-2, then dissolve the white solid in absolute ethanol, add ammonia water and ammonium chloride until the pH is 7-8, and obtain the crude product of diammonium glycyrrhizinate. Firstly heat 80% acetic acid, then add the crude product of diammonium glycyrrhizinate into 80% acetic acid, heat to reflux, after the solution is clear, add activated carbon to decolorize, filter, and the filtrate is still for crystallization. Then the obtained crystals were recrystallized through 75% ethanol according to the previous method to obtain diammonium glycyrrhizinate fine work (content 98.8%, 99.6%) with better quality.

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 diammonium glycyrrhizinate salt preparation method. According to the method, according to the special physical and chemical properties of glycyrrhizic acid, the diammonium glycyrrhizinate salt with characteristics of good color, good character, high content and meeting of the industry standard is produced by using an ammonium glycyrrhizinate salt as a raw material. Compared to the method in the prior art, the method of the present invention has significant advantages of novel process, simple operation, energy saving, environmental protection, strong practicality, mild reaction condition, high conversion rate, easy quality control, reduction of the use of other solvents, reduction of impurity introduction, good product color, simple operation process, low equipment and material cost, high treatment capacity, good product chrominance, good product yield, high content, excellent product color, uniform crystal and good quality, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of compound preparation, in particular to a preparation method of diammonium glycyrrhizinate. Background technique [0002] Diammonium Glycyrrhizinate (Diammonium Glycyrrhizinate) molecular formula: C42H68N2O16, white crystalline powder, odorless, sweet taste, has strong anti-inflammatory, liver cell membrane protection and liver function improvement effects. Prevent the increase of serum ALT caused by ammonium galactose and carbon tetrachloride, and improve the damage of liver tissue. It has become a new type of drug for liver protection and liver protection. Glycyrrhizic acid in nature exists in two configurations, 18α-H and 18β-H. The α-body has a stronger anti-inflammatory effect than the β-body, with high liver targeting, less adverse reactions, and strong safety. It is more suitable for clinical treatment of liver diseases. treat. [0003] At present, the synthesis method of diammonium glycyrrhizinate is gener...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 季浩魏民窦长清阚建伟于燕燕
Owner JIANGSU TIANSHENG PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com