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Method for synthesizing 3',4',7-troxerutin

A trihydroxyethyl rutin, hydroxyethylation technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problem of high impurities, low trihydroxyethyl rutin content, and reaction end Difficult to precisely control and other problems, to achieve the effect of increasing the content of active ingredients

Inactive Publication Date: 2012-02-15
山西津华晖星制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention provides a synthetic 3′, 4′, 7-trihydroxyethyl rutin in order to solve the existing problems of difficult and precise control of the reaction end point, low content of trihydroxyethyl rutin, and many impurities in the existing method for synthesizing 3′, 4′, 7-trihydroxyethyl rutin. , 4', the method of 7-trihydroxyethyl rutin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] A method for synthesizing 3', 4', 7-trihydroxyethyl rutin, which uses rutin and oxirane to carry out hydroxyethylation reaction under the condition that sodium hydroxide is a catalyst, and 500kg purified water , put 2kg of sodium hydroxide into the reactor and stir, add 200kg of rutin, seal the reactor, react under pressure, keep the pressure of the kettle ≤ 0.2Mpa, start adding ethylene oxide when the temperature rises to 50-80°C, and add ethylene oxide every hour The amount of alkane is 4% of the weight of rutin, that is, the adding speed of ethylene oxide is 8kg / h, and now the pH value of the reaction solution is less than 9.5-9.6; Ammonium bicarbonate of acid salt, the addition amount is 0.5% of rutin weight, namely 1kg; When the pH value of the reaction solution is greater than 9.5 to 9.6, reduce the speed of adding ethylene oxide, and add ethylene oxide every hour during this process The amount of rutin is 2.5% of the weight of rutin, that is, the addition rate of...

Embodiment 2

[0011] A method for synthesizing 3', 4', 7-trihydroxyethyl rutin, which uses rutin and oxirane to carry out hydroxyethylation reaction under the condition that sodium hydroxide is a catalyst, and 380kg purified water , put 4.75kg of sodium hydroxide into the reactor and stir, add 95kg of rutin, seal the reactor, react under pressure, keep the pressure of the kettle ≤ 0.2Mpa, start adding ethylene oxide when the temperature rises to 80°C, and add ethylene oxide every hour The amount of rutin is 5% of the weight of rutin, that is, the addition rate of ethylene oxide is 4.75kg / h, and the pH value of the reaction solution is less than 9.5-9.6 at this time; when the pH value of the reaction solution rises to 9.5-9.6, add weak The sodium bicarbonate of acid salt, the addition is 5% of rutin weight, is 4.75kg; When the pH value of reaction solution is greater than 9.5~9.6, reduce the speed of adding ethylene oxide, add epoxy ethane every hour in this process The amount of ethane is 3...

Embodiment 3

[0013] A method for synthesizing 3', 4', 7-trihydroxyethyl rutin, which uses rutin and oxirane to carry out hydroxyethylation reaction under the condition that sodium hydroxide is a catalyst, and 670kg of purified water , put 2.8kg of sodium hydroxide into the reactor and stir, add 225kg of rutin, seal the reactor, react under pressure, keep the pressure of the kettle ≤ 0.2Mpa, start adding ethylene oxide when the temperature rises to 60°C, and add ethylene oxide every hour The amount of rutin is 5% of the weight of rutin, that is, the addition rate of ethylene oxide is 11.25kg / h, and the pH value of the reaction solution is less than 9.5-9.6 at this time; when the pH value of the reaction solution rises to 9.5-9.6, the addition is weak The ammonium carbonate of acid salt, the addition is 3% of rutin weight, is 6.75kg; When the pH value of reaction liquid is greater than 9.5~9.6, reduce the speed of adding ethylene oxide, add ethylene oxide every hour in this process The amoun...

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Abstract

The invention relates to the field of chemical pharmacy, in particular to a method for synthesizing 3',4',7-troxerutin, and solves the problems that a reaction end point has the characteristics of not easy control, low content, various impurities and the like in a conventional synthesizing method. In the method, rutin reacts with epoxy ethane by taking sodium hydroxide as a catalyst, wherein the weight ratio of the rutin to the epoxy ethane is 1:2 to 1:4; the weight ratio of the rutin to the sodium hydroxide is 100:1-100:1.5; before the pH value of reaction solution reaches 9.5 to 9.6 and when the reaction temperature is between 50 and 80 DEG C, the additive amount of the epoxy ethane per hour is 4 to 5 percent based on the weight the rutin; after the pH value of the reaction solution reaches 9.5 to 9.6 and when the reaction temperature is between 40 and 70 DEG C, the additive amount of the epoxy ethane is 2.5 to 3.5 percent based on the weight of the rutin; and when the pH value of the reaction solution is 9.5 to 9.6, a weak acid salt is added. The content of the troxerutin is stabilized over 78 percent while an obtained product has very few impurities, so that national medicament standards can be reached without refining; and therefore, method improves the yield by 125 to 130 percent, reduces production cost, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of chemical pharmacy, in particular to a method for synthesizing 3', 4', 7-trihydroxyethyl rutin. Background technique [0002] Troxerutin is a water-soluble product obtained by hydroxyethylation of rutin, which has better in vivo absorption and more significant curative effect than rutin, among which 3′,4′,7-trihydroxyethyl rutin As the main ingredient, it also has the greatest curative effect. Troxerutin has the functions of reducing capillary permeability and fragility, improving capillary resistance, inhibiting platelet aggregation, and preventing thrombosis. It can be used clinically to treat cerebral thrombosis and hemiplegia and aphasia caused by cerebral thrombosis. Arteriosclerosis, varicose veins, central retinitis, pre-myocardial infarction syndrome, and edema caused by high vascular permeability are especially effective in preventing arteriosclerosis. The current commonly used preparation process of trox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/00C07H17/07
Inventor 于海勇高谦常德才董永杰马菁
Owner 山西津华晖星制药有限公司
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