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Preparation method of myricetin

A technology of myricetin and dihydromyricetin, applied in the direction of organic chemistry, etc., to achieve the effects of simple operation, low cost and high product yield

Active Publication Date: 2016-02-03
SHAANXI JIAHE PHYTOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN101973976 reports a method for extracting dihydromyricetin from vine tea; patent CN03138054 reports a method for extracting dihydromyricetin and myricetin composition from vine tea; patent CN1887881 reports using vine tea as raw material Water extraction, concentration, adding a weak base, the conversion of dihydromyricetin into myricetin, the yield is only 8%

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  • Preparation method of myricetin
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preparation example Construction

[0016] The semi-synthetic method of myricetin of the present invention comprises following synthetic route:

[0017]

Embodiment 1

[0019] In a four-necked reaction flask, feed 20 g of dihydromyricetin, 200 ml of ethanol with a mass concentration of 85%, stir evenly, add dropwise 13 ml of sodium hypochlorite solution with a mass concentration of 10%, 1 g of anhydrous ferric chloride, and heat up to reflux for 2 h Finally, add 2ml of sodium hypochlorite solution with a mass concentration of 10%, and continue to reflux. After 2h, TLC detects that the reaction of the raw materials is complete, and the reaction is stopped. It is cooled to room temperature, left overnight, filtered, and dried at 60°C to obtain 17g of yellow needle-shaped solids. Content 98% (HPLC), yield 85.5%.

Embodiment 2

[0021] In a four-necked reaction flask, feed 20 g of dihydromyricetin, 260 ml of ethanol with a mass concentration of 90%, stir well, add dropwise 12 ml of sodium hypochlorite solution with a mass concentration of 10%, 1 g of anhydrous ferric chloride, and heat up to reflux for 1 h Finally, add 2.5ml of sodium hypochlorite solution with a mass concentration of 10%, and continue to reflux. After 2.5 hours, TLC detects that the reaction of the raw materials is complete, stop the reaction, cool down to room temperature, stand overnight, filter, and dry at 60°C to obtain a yellow needle-shaped solid 17.4g. Content 98% (HPLC), yield 87.6%.

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Abstract

The invention provides a preparation method of myricetin. The preparation method comprises the following steps: mixing dihydromyricetin with alcohols, then adding a sodium hypochlorite solution and a catalyst to carry out reactions, and after the reactions, keeping on adding a sodium hypochlorite solution to obtain myricetin; wherein the alcohol is methanol or ethanol, and the catalyst is anhydrous aluminum trichloride or anhydrous iron trichloride. According to the preparation method, dihydromyricetin is taken as the primary raw material, myricetin is prepared from dihydromyricetin through semi-synthesis, dihydromyricetin is extracted from vine tea, the content is 98% or more, the cost is low, the operation is simple, the product yield is high, the product does not need refinement, the content is 98% or more, and the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a semi-synthetic method of natural product myricetin. Background technique [0002] Myricetin, also known as myricetin, chemical name 3, 3, 4, 5, 5, 7-6 hydroxyflavone, pure product is yellow needle-like crystals. Myricetin widely exists in the leaves, roots and branches of bayberry. It has the effects of constricting blood vessels, raising blood pressure, exciting the heart, promoting choleresis, anti-inflammation, and causing mutagenesis. It can also be used to treat diabetes and cataracts. Development research is of great significance. The structural formula of myricetin is as follows: [0003] [0004] The content of myricetin in natural plants is very small, and it is reported in the literature that there are about 2% of the content in natural vine tea and the leaves of the genus Snake Grape of the family Vitis genus, but the plant vine tea is rich in dihydro...

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 肖金霞郭文华张瑜靳莎杨雪峰
Owner SHAANXI JIAHE PHYTOCHEM
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