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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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0011] Because these impurities do not have the pharmacological effects

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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Example Embodiment

[0029] Example 1: Method for preparing troxerutin

[0030] At 75℃, add 100g rutin, 100g water, 0.82g sodium hydroxide into the reaction kettle, and then pass nitrogen to drive off oxygen; then pass ethylene oxide to monitor the pH of the solution, when the pH of the reaction solution is 9.1 When the reaction temperature was lowered to 60° C., 10 g of resin was added, and the reaction was continued until the pH of the reaction solution was 10.0, then the addition of ethylene oxide was stopped. Add 1:1 aqueous hydrochloric acid 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. The content of 3', 4', 7-trihydroxyethyl rutin detected by HPLC is 92.8% .

Example Embodiment

[0031] Example 2: Method for preparing troxerutin

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

Example Embodiment

[0033] Example 3: Method for preparing troxerutin

[0034]At 75°C, 100g rutin, 200g water, 0.85g sodium hydroxide were added to the reaction kettle, and then ethylene oxide was introduced to monitor the pH of the solution. When the pH of the reaction solution was 9.3, the reaction temperature was lowered to At 60° C., add 10 g of resin, continue the reaction until the pH of the reaction solution is 10.2, stop adding ethylene oxide. Add 1:1 aqueous hydrochloric acid 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, of which 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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