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Method for preparing high-content troxerutin drug

A technology of rutin and content, which is applied in the field of preparation of high-content troxerutin medicine, can solve the problem that troxerutin does not have pharmacological effects, and achieve the effect of increasing yield and content

Active Publication Date: 2006-08-09
TOPFOND PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Because these impurities do not have the pharmacological effects of troxerutin, there will be safety hazards when entering the human body

Method used

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  • Method for preparing high-content troxerutin drug
  • Method for preparing high-content troxerutin drug
  • Method for preparing high-content troxerutin drug

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1: the method for preparing troxerutin

[0030] At 75°C, add 100g of rutin, 100g of water, and 0.82g of sodium hydroxide into the reaction kettle, feed nitrogen to drive off oxygen; then feed ethylene oxide, monitor the pH of the solution, when the pH of the reaction solution is 9.1 , lower the reaction temperature to 60° C., add 10 g of resin, and continue the reaction until the pH value of the reaction solution is 10.0, then stop adding ethylene oxide. Add 1:1 hydrochloric acid aqueous solution to adjust the pH value of the solution to about 4.5, hot filter, concentrate, and vacuum-dry to obtain 120.5 g of troxerutin, of which the content of 3', 4', 7-trihydroxyethyl rutin detected by HPLC is 92.8% .

Embodiment 2

[0031] Embodiment 2: the method for preparing troxerutin

[0032] At 75°C, add 100g of rutin, 150g of water, and 0.83g of sodium hydroxide into the reaction kettle, and then feed ethylene oxide to monitor the pH of the solution. When the pH of the reaction solution is 9.2, lower the reaction temperature to At 60°C, 10 g of resin was added, and the reaction was continued until the pH value of the reaction solution was 10.1, then the addition of ethylene oxide was stopped. Add 1:1 hydrochloric acid aqueous solution to adjust the pH value of the solution to about 4.5, hot filter, concentrate, and vacuum-dry to obtain 121.2 g of troxerutin, wherein the content of 3', 4', 7-trihydroxyethyl rutin detected by HPLC is 85.2% .

Embodiment 3

[0033] Embodiment 3: the method for preparing troxerutin

[0034]At 75°C, add 100g of rutin, 200g of water, and 0.85g of sodium hydroxide into the reaction kettle, and then feed ethylene oxide to monitor the pH value of the solution. When the pH value of the reaction solution is 9.3, reduce the reaction temperature to At 60°C, 10 g of resin was added, and the reaction was continued until the pH value of the reaction solution was 10.2, then the addition of ethylene oxide was stopped. Add 1:1 hydrochloric acid aqueous solution to adjust the pH value of the solution to about 4.5, hot filter, concentrate, and vacuum-dry to obtain 120.4 g of troxerutin, wherein the content of 3', 4', 7-trihydroxyethyl rutin detected by HPLC is 81.6% .

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Abstract

The invention offers 3', 4', 7-troxerutin synthetic method. It uses rutin and ethylene oxide to do hydroxyethylation reaction under the catalyzing of sodium hydroxide. Its features are that in the reaction, the weight ratio of rutin and water is 1:1-1:3; optimization is 1:1-1:1.5; the weight ratio of rutin and sodium hydroxide is 100:0.82-100:0.85; adding resin when the pH value of the reaction solution is 9.0-9.5 to adjust end point pH value to 9.5-10.3. The method can make high purity and high quality troxerutin. And its 3', 4', 7-troxerutin content is more than 78%; optimization is more than 80%; and the more optimization is more than 85%.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy, in particular, the invention relates to a preparation method of troxerutin medicine with high content. Background technique [0002] The chemical name of Troxerutin is: 3', 4', 7-tri[O-(2-hydroxyethyl)] rutin, referred to as 3', 4', 7-trihydroxyethyl rutin Ding, a water-soluble product obtained by hydroxyethylation of rutin, has better absorption and better curative effect than rutin, can reduce capillary permeability and fragility, improve capillary resistance, inhibit Platelet aggregation, prevention of thrombosis, etc., can be used to treat hemiplegia, aphasia, arteriosclerosis, varicose veins, central retinitis, pre-myocardial infarction syndrome, and edema caused by increased vascular permeability caused by cerebral thrombosis and cerebral embolism and other diseases, especially in the prevention of arteriosclerosis has a good effect. [0003] CN1056850C discloses a method for synthesizing...

Claims

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Application Information

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IPC IPC(8): C07H17/07A61K31/7048
Inventor 王伟王辉刘金平周新建马国旺王俊臣杜舒文吴总社
Owner TOPFOND PHARMA CO LTD
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