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Diammonium glycyrrhizinate salt preparation method

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

Active Publication Date: 2017-03-08
JIANGSU TIANSHENG PHARMA
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  • 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

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Combine 300g of glycyrrhizinate monoammonium salt and 1500ml of 25% sodium hydroxide solution, heat to 90°C and reflux for 12h, and after falling to 0°C, adjust the pH to 1-2 with 40% hydrochloric acid solution; keep it warm for 1h and filter to get White solid; washed twice with an aqueous hydrochloric acid solution with a pH of 1-2, then dissolve the white solid in absolute ethanol, add ammonia and ammonium chloride to a pH of 7-8 to obtain crude diammonium glycyrrhizinate. The crude diammonium glycyrrhizinate was added to 85% acetic acid, heated to reflux, and after the solution was clear, activated carbon was added for decolorization, filtered, and the filtrate was statically crystallized. Then, the obtained crystals were recrystallized with 80% ethanol according to the previous method to obtain a fine quality diammonium glycyrrhizinate (content 98.5%, 99.4%).

Embodiment 2

[0025] Combine 300g of glycyrrhizinate monoammonium salt and 1500ml of 30% sodium hydroxide solution, heat to 90°C and reflux for 12h, then adjust the pH to 1-2 with 30% hydrochloric acid solution after falling to 0°C; keep it warm for 1h and filter to obtain white Solid; washed twice with a hydrochloric acid aqueous solution with a pH of 1-2, then dissolve the white solid in absolute ethanol, add ammonia and ammonium chloride to a pH of 7-8 to obtain crude diammonium glycyrrhizinate. The crude diammonium glycyrrhizinate was added to 80% acetic acid and heated to reflux. After the solution was clear, activated carbon was added for decolorization, filtered, and the filtrate was statically crystallized. Then, the obtained crystals were recrystallized with 75% ethanol according to the previous method to obtain a fine quality diammonium glycyrrhizinate (content 98.5%, 99.4%).

Embodiment 3

[0027] Combine 300g of glycyrrhizinate monoammonium salt and 1500ml of 30% sodium hydroxide solution, heat to 90°C and reflux for 12h, then adjust the pH to 1-2 with 30% hydrochloric acid solution after falling to 0°C; keep it warm for 1h and filter to obtain white Solid; washed twice with a hydrochloric acid aqueous solution with a pH of 1-2, then dissolve the white solid in absolute ethanol, add ammonia and ammonium chloride to a pH of 7-8 to obtain crude diammonium glycyrrhizinate. The 80% acetic acid is heated first, and then the crude diammonium glycyrrhizinate is added to the 80% acetic acid, heated to reflux, after the solution is clear, activated carbon is added for decolorization, filtered, and the filtrate is statically crystallized. Then, the obtained crystals were recrystallized with 75% ethanol according to the previous method to obtain a fine quality diammonium glycyrrhizinate (content 98.8%, 99.6%).

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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 method for preparing diammonium glycyrrhizinate. Background technique [0002] Diammonium Glycyrrhizinate (Diammonium Glycyrrhizinate) molecular formula: C42H68N2O16, white crystalline powder, odorless, sweet taste, has a strong anti-inflammatory, protect liver cell membrane and improve liver function. It prevents the increase in serum ALT caused by ammonium galactose and carbon tetrachloride, and improves liver tissue damage. It has become a new type of liver protection and liver protection. Glycyrrhizic acid in nature exists in two configurations of 18α-H body and 18β-H body. α-body has stronger anti-inflammatory effect than β-body, high liver targeting, low side effects, and strong safety. It is more suitable for clinical liver disease treatment. [0003] At present, the synthesis method of diammonium glycyrrhizinate is generally to extract glycyrrhizic acid from licorice with...

Claims

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Application Information

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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
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