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Clean preparation process of high-purity hesperetin

A preparation process, the technology of hesperetin, which is applied in the field of clean preparation process of high-purity hesperetin, can solve the problems of high cost, unsuitable for industrial production, complicated steps, etc.

Inactive Publication Date: 2013-06-19
李玉山
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of total synthesis is low, the cost is high, and the steps are complicated, so it is not suitable for industrial production
Shen Jing and others used hesperidin as a raw material and converted it into hesperetin with glucosidase, which did not have the conditions for industrialization

Method used

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  • Clean preparation process of high-purity hesperetin

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Comparison scheme
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Embodiment Construction

[0013] Close the mouth of the reaction kettle, vacuum pump 1300kg of 99% methanol with accurate measurement into the reaction kettle, open the mouth of the reaction kettle, start stirring, adjust the pH of the methanol solution to 1-2 with concentrated sulfuric acid, add 1.0-1.5% vitamin C, and slowly add it from the mouth of the reaction kettle Hesperidin 200.0kg, seal the reaction kettle mouth, open the heat-carrying steam valve of the reaction kettle to heat, close the heat-carrying steam valve when the pressure indicated by the pressure gauge on the reaction kettle reaches 0.22MPa, start timing when the pressure rises to 0.25MPa, and maintain the pressure in the kettle At 0.22~0.25Mpa5~7h. After the reaction was complete, the pressure was lowered to obtain a clear and translucent hesperetin reaction solution. The reaction solution was concentrated under reduced pressure at 50°C, and the concentration was stopped after the alcohol content of the concentrated solution reache...

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Abstract

The invention relates to a clean preparation process of high-purity hesperetin. The process mainly comprises the following steps: (1) hydrolyzing hesperidin to obtain the hesperetin, (2) concentrating hesperetin reaction liquid in a vacuum mode, (3) depositing the hesperetin concentrated solutions, (4) preparing the hesperetin, and (5) processing filter pressing acid water solutions. According to the process, hesperetin which is more than 95% in content (high performance liquid chromatography (HPLC)) is obtained through a further reaction and a special processing process. Compared with the facts that in prior art, a crude product is firstly obtained through hydrolyzing, and then a fine product is obtained by refining the crude product, the clean preparation process of high-purity hesperetin has the advantages of being simple in process, low in cost, and high in yield. Acid water which is generated by hydrolyzing is well processed and recycled, rhamnose in the acid water is abstracted, and crystallization mother liquor is prepared into agricultural nucleic acid. Therefore, the whole production process is resource-saving and environment-friendly.

Description

technical field [0001] The invention relates to a clean preparation process of high-purity hesperetin. Background technique [0002] Hesperidin, which is off-white fine powder, belongs to flavonoids. Alias: 5,7,3'-trihydroxy-4'-methoxyflavanone, eriodictol 4'-methyl ether. Molecular formula C 16 h 14 o 6 ; Molecular weight 302.29. Melting point 226-228℃, easily soluble in methanol, ethanol, acetone and other organic solvents, soluble in dilute alkali solution, partially soluble in ether. Insoluble in water (273mg / L). Slightly soluble in chloroform and benzene. The plants are derived from sweet orange Citrus sinensis and lemon Citrus limon, which belong to the genus Citrus of Rutaceae. It may also exist in the aboveground part of Rubiaceae plant Chestnut chinensis; Rutaceae plant bergamot fruit, banana orange fruit, citrus fruit, lemon fruit, quinoa lemon peel, citron ripe fruit; Cruciferous plant shepherd's purse, whole plant with roots . The structural formula is ...

Claims

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Application Information

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IPC IPC(8): C07D311/32C07H3/08C07H1/00
Inventor 李玉山
Owner 李玉山
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