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New technology for preparing luteolin by using hesperidin

A technology of luteolin and hesperidin, applied in the direction of organic chemistry, etc., can solve the problems of cumbersome process, low yield and low output

Inactive Publication Date: 2013-06-12
李玉山
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] There are currently four methods for preparing luteolin: 1) plant extraction, extracting from plants containing luteolin, and obtaining luteolin through separation and purification, the yield is not high, and the process is cumbersome
2) Total synthesis, phloroglucinol and ethyl 3,4-dimethoxybenzoylacetate are synthesized, and the obtained intermediate is demethylated to obtain crude luteolin, which is washed and recrystallized to obtain luteolin Vegetarian pure product, the yield of this method is low
This method is relatively complicated and has not yet been industrialized

Method used

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  • New technology for preparing luteolin by using hesperidin
  • New technology for preparing luteolin by using hesperidin

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Embodiment Construction

[0017] Preparation of the first hesperidin: close the mouth of the reaction kettle, pump 1500-1700Kg of ethanol with accurate measurement into the reaction kettle, the ethanol has been adjusted to pH 1-2 with concentrated sulfuric acid, slowly add 120Kg of crude hesperidin from the reaction kettle mouth, and seal the reaction At the kettle mouth, start stirring, open the heat-carrying steam valve of the reaction kettle to heat, open the circulating condensed water, and reflux at 70-75°C for reaction. After reacting for 12 hours, take a sample from the sampling port for detection. After the reaction is complete, start to concentrate until the purity of the concentrated solution reaches 15-25%. ℃ dry 4 ~ 8h. Obtain the crude product of hesperetin. Add 900Kg of 95% ethanol to the reaction kettle, put 100Kg of crude hesperetin into it, then add 3kg of activated carbon, close the mouth of the kettle, open the heat carrying steam valve of the reaction kettle, and wait until the tem...

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Abstract

The invention provides new technology for preparing luteolin by using hesperidin. The method includes a first step of hydrolyzing hesperidin to obtain hesperetin, a second step of dehydrogenizing the hesperetin to obtain diosmetin, and a third step of demethylating the diosmetin to obtain the luteolin. Compared with the prior art that the hesperidin is firstly dehydrogenized and then hydrolyzed, the method enables iodine using amount to be greatly reduced, and production cost is low. The invention further provides new technology for preparing the diosmetin.

Description

technical field [0001] The invention relates to a new technology for preparing luteolin from hesperidin. Background technique [0002] Luteolin (Luteolin), chemical name: 3', 4'5, 7-tetrahydroxyflavone, alias: yellow flavin, Huang Shiling, chemical formula: C 15 h 10 o 6 , molecular weight: 286.23. Yellow needle-like crystal, melting point 328-330°C, slightly soluble in water, slightly acidic, soluble in alkaline solution. The structural formula is as follows: [0003] [0004] Luteolin is widely distributed in nature and is named after it was originally isolated from the leaves, stems and branches of the herb Resedaodorata L. in the family Resedaceae. Mainly from the shell of the fruit of the leguminous plant Arachis hypogata L., the labiatae plant Ajugadecumbens Thunb., the Gentianaceae plant Gentianopsis palucisa (Munro) Ma), the Patraceae plant black Water valerian (Valeriana amurensis P.Smirn.) aerial part and Lonicera japonica Thunb. etc. At present, it is al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30
Inventor 李玉山
Owner 李玉山
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