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Method for synthesizing luteolin

A technology of luteolin and ethanol, which is applied in the synthesis field of preparing luteolin, can solve the problems of low extraction rate, and achieve the effects of high synthesis efficiency, high yield, and easy industrial production

Active Publication Date: 2012-08-22
西安炎黄经方医药研发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Luteolin is the same active ingredient isolated from whole-leaf Qinglan and Anhui Prunella vulgaris, the extraction rate in the prior art is very low, 2 / 10,000, and its structure is 3', 4', 5, 7-4 Hydroxyisoflavones

Method used

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  • Method for synthesizing luteolin

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Effect test

Embodiment 1

[0016] synthetic route:

[0017]

[0018] Preparation: Add 600 grams of water to a 1L three-necked bottle, then add 90 grams of sodium hydroxide, stir to dissolve it, wait until the temperature of the reaction bottle drops to 20-30 degrees, slowly add 30 grams of rutin, and continue stirring for 30 Minutes, until the rutin is completely dissolved, then heat up to 50 degrees, add 65 grams of sodium hydrosulfite, stir at this temperature for 45 minutes, heat up to 100 degrees, and stir for 12 hours. HPLC detects that the reaction is over, cool the reaction bottle, drop dilute hydrochloric acid or dilute sulfuric acid between 20-25 degrees, adjust the pH to 3-4, then let it stand for 10 hours, filter, wash with water, and dry to obtain 11.5 grams of crude Osmanthus osmanthus Grass.

[0019] Refining: Add 11.5 grams of crude luteolin to 200 grams of ethanol, heat to dissolve, then concentrate to get 120 grams of ethanol, place the remaining solution at 0-10 degrees for 8 hours...

Embodiment 2

[0021] Preparation: Clean the 500L glass-lined reaction kettle, add 300kg of water to the kettle, then add 45kg of caustic soda, turn on the cooling water to lower the temperature to below 25 degrees, add 15kg of rutin in 3 batches, and then stir for 1 Hours to dissolve all the rutin. Then heat up to 45-50 degrees, slowly add 32.5 kg of hydrochloric acid, stir at this temperature for 30 minutes, then heat up to reflux for 12 hours, cool the reactor to below 20 degrees, drop dilute hydrochloric acid until the pH reaches 3-4, and then Let it stand for 10 hours, pass through plate and frame filter press, wash the product obtained once with water, and dry to obtain 6 kg of luteolin.

[0022] Refining: dissolving 6 kg of luteolin in 100 kg of ethanol, then steaming out 55 kg of ethanol, cooling the remaining solution to 0-5 degrees, standing for 10 hours for crystallization, and obtaining 4 kg of luteolin with a purity of 95.6% , the yield was 56.5%.

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Abstract

The invention discloses a method for synthesizing luteolin, comprising the following steps of: adding rutin at the room temperature of 20-30DEG C in alkali water and stirring for dissolving; adding a reducing agent of sodium hydrosulfite with equivalent weight of 6.3 once, continuously heating up to 100DEG C and stirring for 12 hours; after the HPLC (High Performance Liquid Chromatography) monitoring reaction is finished, cooling, adding dilute hydrochloric acid or dilute sulfuric acid, adjusting the pH to be 3-4, standing for 24 hours for separating out a solid and filtering; washing a filtering cake with water twice to remove salts contained in the product; and drying to obtain a crude product, continuously crystalizing with ethanol to obtain a pure product with the purity being more than 95 percent. Compared with the prior art, the invention has the advantages of high synthetic efficiency, high yield, low energy consumption, low pollution, greenness, environmental protection and the like and is easy for industrialized production.

Description

technical field [0001] The invention relates to the field of substance synthesis, in particular to a synthesis method for preparing luteolin from natural extracts. Background technique [0002] Luteolin is the same active ingredient isolated from whole-leaf Qinglan and Anhui Prunella vulgaris, the extraction rate in the prior art is very low, 2 / 10,000, and its structure is 3', 4', 5, 7-4 Hydroxyisoflavones. According to reports, this product has a good curative effect on inflammation, tumor, allergy and inflammatory demyelinating diseases. It can also inhibit a variety of viruses. It has been used clinically and made into medicine. Therefore, luteolin has a broad market prospect. Contents of the invention [0003] The object of the present invention is to provide a new method for synthesizing luteolin with rutin as raw material through one-step chemical reaction. [0004] The specific process of this method is to add rutin into alkaline water at a temperature of 20-30...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/30
Inventor 王超
Owner 西安炎黄经方医药研发有限公司
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