Preparation method of high-content troxerutin

A high-content, rutin technology, applied in the field of high-content troxerutin preparation, can solve the problems of complicated operation, high cost, unsuitable for industrialization promotion and application, etc.

Active Publication Date: 2018-08-03
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010]In the existing reports, the only method for troxerutin content to reach 98.0% or more is chromatography,

Method used

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  • Preparation method of high-content troxerutin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Add 152g (0.25mol) of crude rutin to 750mL of pyridine, stir until dissolved, slowly drop in 305g (3mol) of acetic anhydride in an ice-water bath, stir at 70°C for 12h, then drop the reaction solution into 15L In the ice water solution, milky white particles were precipitated. After static crystallization at room temperature for 4 hours, filter with suction; heat the filter cake with 2.5L isopropanol until dissolved, add 15.2g of equal mass boric acid and activated carbon mixture, filter while hot, and then Slowly lower the temperature to crystallize, and filter with suction; dissolve the filter cake in 1L of methanol, and then slowly add 160g (3mol) of sodium methoxide in methanol solution dropwise. , a large amount of yellow precipitates were precipitated, left standing at room temperature, and suction filtered to obtain high-content rutin, with a yield of 95.4% and a purity of 99.7%;

[0030] (2) get 145g rutin and 7.2g 3 generations of PAMAM dendrimers obtained ...

Embodiment 2

[0033] (1) Add 152g (0.25mol) of crude rutin to 750mL of pyridine, stir until dissolved, slowly drop in 305g (3mol) of acetic anhydride in an ice-water bath, stir at 70°C for 12h, then drop the reaction solution into 15L In the ice water solution, milky white particles were precipitated. After static crystallization at room temperature for 4 hours, suction filtration; the filter cake was heated to dissolve with 2.5L ethyl acetate, and 12.5g equal mass of boric acid and activated carbon mixture was added, while hot suction filtration, and then Drop into 2.5L of petroleum ether, slowly cool down and crystallize, and filter with suction; dissolve the filter cake in 1L of methanol, and then slowly add 160g (3mol) of methanol solution of sodium methoxide dropwise to it, at this time the solution becomes cloudy, adjust with glacial acetic acid The pH value of the mixed system was 5.8, and a large amount of yellow precipitates precipitated out. After standing at room temperature, high...

Embodiment 3

[0037] (1) Add 152g (0.25mol) of crude rutin into 750mL of triethylamine, stir until dissolved, slowly drop in 235g (3mol) of acetyl chloride in an ice-water bath, stir at 70°C for 12h, and dissolve the reaction solution Drop into 15L of ice water solution, milky white particles precipitate out, stand at room temperature for crystallization for 4 hours, then suction filter; heat the filter cake with 2.5L of ethyl acetate until dissolved, add 15.2g of equal mass boric acid and activated carbon mixture, and pump while hot Filter, then slowly cool down and crystallize, and suction filter; dissolve the filter cake in 1L methanol, and slowly add 160g (3mol) methanol solution of sodium methoxide dropwise to it, at this time the solution becomes cloudy, adjust the pH of the mixed system with dilute hydrochloric acid The value was 6.0, and a large amount of yellow precipitates were precipitated. After standing at room temperature, high-content rutin was obtained by suction filtration, ...

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Abstract

The invention discloses a preparation method of high-content troxerutin and belongs to the technical field of pharmaceutical chemistry. The preparation method is characterized in that the preparationmethod of high-content troxerutin comprises the following steps: carrying out acetylation and purification of crude rutin used as a raw material, then hydrolyzing the crude rutin to obtain high-content rutin with a content being higher than 99.0%; reacting the high-content rutin under the catalysis action of a catalyst which is a third-generation PAMAM dendrimer to prepare troxerutin; and purifying the troxerutin to obtain the high-content troxerutin with a content being higher than 99.0%. According to the method, the high-quality rutin with the content being higher than 99.0% is used as the raw material, so that the high-content troxerutin crude drug is prepared; the method is low in cost and simple and convenient in steps, is economical and environmentally friendly, and is suitable for industrial production; the content of the prepared troxerutin can reach 99.0% or above.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a preparation method of high-content troxerutin. Background technique [0002] Troxerutin is 7,3′,4′-trihydroxyethylrutin, this product is light yellow or light yellow green powder, molecular formula is C 33 h 42 o 19 , CAS No. 7085-55-4, molecular weight 742.68, melting point 168-176°C, its structural formula is as follows: [0003] [0004] Troxerutin is a class of anticoagulant and thrombolytic drugs, it can inhibit platelet aggregation, prevent thrombosis, and at the same time resist vascular damage caused by 5-hydroxytryptamine and bradykinin, and increase capillary resistance , reduce capillary permeability, prevent edema caused by increased vascular permeability, and have a significant protective effect on acute ischemic brain injury. [0005] Troxerutin is prepared by using rutin and ethylene oxide as raw materials, and undergoes Williamson ...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/00
CPCC07H1/00C07H17/07
Inventor 姜玉钦李阳李言言张玮玮李星徐桂清李伟
Owner HENAN NORMAL UNIV
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