Preparation method of anhydroicaritin

A technology of icariin and icariin, applied in the direction of organic chemistry, can solve the problems of high enzymatic hydrolysis cost, high cost, harsh conditions, etc., and achieve simple and easy operation, low environmental pressure, and mild conditions Effect

Pending Publication Date: 2019-07-09
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yields are not high, and the cost of enzymatic hydrolysis is relatively high; the yield of the chemical synthesis method is also low, the conditions are relatively harsh, and the distance from industrialization is relatively long
At present, these preparation methods have limited their large-scale production and application in industry due to reasons such as small yield, low yield, and high cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) smith degradation Add 2g of icariin to 5% ethanol aqueous solution to prepare a solution with icariin content of 0.001mol / L, add acetic acid to adjust the pH to 5.0, and the molar ratio of icariin to oxidant is 1 : 4 Add sodium periodate to the solution, and after 72 hours of dark reaction at room temperature, add glycerin to stop the oxidation, add sodium hydroxide solution to adjust the pH to neutral, concentrate to no alcohol smell, and use an equal volume of ethyl acetate The ester was extracted 3 times, the extracts were combined, concentrated to dryness, and the oxidized product was obtained; the oxidized product was dissolved in 50% ethanol aqueous solution, and the mass ratio of the added 50% ethanol aqueous solution to icariin was 40:1, and then hydroboration was added Sodium, the molar ratio of sodium borohydride and icariin is 4:1, after 72 hours of reaction, the reaction is terminated; 1.2mL of 36% hydrochloric acid is added to the reduction reaction solu...

Embodiment 2

[0030] (1) smith degradation Add 2g of icariin to 20% ethanol aqueous solution to prepare a solution with icariin content of 0.02mol / L, add acetic acid to adjust the pH to 4.0, and the molar ratio of icariin to oxidant is 1 : 6 Add potassium periodate to the solution, react in the dark at room temperature for 48 hours, then add glycerin to stop the oxidation, add sodium carbonate to adjust the pH to neutral, concentrate to no alcohol smell and then extract with an equal volume of ethyl acetate 3 times, the combined extracts were concentrated to dryness to obtain the oxidation product; the oxidation product was added to 70% ethanol aqueous solution, and the mass ratio of the added 70% ethanol aqueous solution to icariin was 20:1; then potassium borohydride, potassium borohydride The molar ratio to icariin is 6:1, and after 48 hours of reaction, the reduction reaction is terminated; 5.4 mL of 5% sulfuric acid is added to the reduction reaction solution, and stirred at 40° C. for ...

Embodiment 3

[0034] (1) smith degradation Add 2g of icariin to 50% ethanol aqueous solution to prepare a solution with icariin content of 0.08mol / L, add acetic acid to adjust the pH to 3.9, and the molar ratio of icariin to oxidant is 1 :10 Add sodium periodate in the solution, after 12 hours of dark reaction under room temperature condition, add glycerin to stop oxidation, add sodium bicarbonate to adjust PH to neutrality, be concentrated to the ethyl acetate of equal volume after being concentrated to no alcohol smell Extract 3 times, combine the extracts, concentrate to dryness to obtain the oxidation product; add the oxidation product to 90% ethanol aqueous solution, the mass ratio of the added 90% ethanol aqueous solution to icariin is 10:1; then add sodium borohydride, boron The molar ratio of sodium hydride to icariin is 8:1, and after 36 hours of reaction, the reduction reaction is terminated; 8 mL of 5% nitric acid is added to the reduction reaction liquid, and stirred at 60° C. fo...

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Abstract

The invention discloses a preparation method of anhydroicaritin. According to the method, icariin is used as a raw material, and high-purity anhydroicaritin is prepared through smith degradation and purification. According to the method, anhydroicaritin is prepared by adopting the smith degradation method for the first time, the problem of structure change caused by acid hydrolysis is effectivelysolved, the method is simple to operate, mild in condition, high in product quality and low in cost, and the requirement of industrial production of anhydroicaritin is met.

Description

technical field [0001] The invention relates to a preparation method of icariin, which belongs to the field of traditional Chinese medicine extraction. Background technique [0002] Epimedium is a plant of the Berberidaceae family, also known as three-branch nine-leaf grass, fairy spleen, etc. It is an important Chinese medicinal material and has a medicinal history of more than two thousand years in my country. "Compendium of Materia Medica" records that Epimedium has the effects of "replenishing the waist and knees, strengthening the bones and bones, helping the yang and improving the essence". Modern pharmaceutical experimental studies have shown that icariin is its main active ingredient, and icariin has stronger pharmacological activity than icariin and icariin in many aspects. Icariin mainly has estrogen-like properties, immune regulation, anti-inflammation, promotion of cardiomyocyte regeneration and differentiation, promotion of bone protection, promotion of nerve c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
CPCC07D311/30C07D311/40
Inventor 张贵民陈小荣韩廷伟
Owner LUNAN PHARMA GROUP CORPORATION
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