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Preparation method of high-purity naringenin

A technology for naringenin and naringenin is applied in the field of preparation of naringenin to achieve the effects of mild reaction conditions, easy operation and high practical value

Inactive Publication Date: 2012-05-16
HENAN TOPFOND PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN1555793A also discloses a method for preparing naringenin by hydrolyzing naringenin, but this method also requires multiple crystallizations to obtain naringenin with higher purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dissolve 6kg of naringin in 20kg of methanol and stir for 30 minutes at room temperature. Cool down to 0°C, add a certain amount of concentrated hydrochloric acid dropwise, adjust the pH value to 2.5, and control the temperature at 0-15°C during the dropwise addition.

[0021] After the dropwise addition, the temperature was gradually raised to 70° C., and the reaction was stirred for 38 hours.

[0022] Methanol was removed under reduced pressure to obtain crude naringenin.

[0023] Add 20kg of absolute ethanol to the obtained crude naringenin, heat to 52°C, and dissolve until clear. Add 300 grams of activated charcoal; stir for 1 hour.

[0024] Filter off activated carbon, then add 20kg of purified water, cool to normal temperature and crystallize for 36 hours.

[0025] Suction filtration, rinse the filter cake with an appropriate amount of absolute ethanol, and dry in a vacuum oven at 60°C for 2 hours. 1.64 kg of white or off-white needle crystals were obtained. ...

Embodiment 2

[0028] Dissolve 10kg of naringin in 34kg of ethanol and stir for 20 minutes at room temperature. Cool down to 0°C, add a certain amount of concentrated hydrochloric acid dropwise to adjust the pH value to 3.0, and dropwise control the temperature at 0-15°C.

[0029] After the dropwise addition, the temperature was gradually raised to 75° C., and the reaction was stirred for 40 hours.

[0030] Ethanol was removed under reduced pressure to obtain crude naringenin. Add 35kg of absolute ethanol to the obtained crude naringenin, heat to 50°C, and dissolve until clear. Add 400 grams of activated charcoal; stir for 1 hour.

[0031] Filter off activated carbon, then add 35kg of purified water, cool to room temperature and crystallize for 40 hours.

[0032] Suction filtration, rinse the filter cake with an appropriate amount of absolute ethanol, and dry in a vacuum oven at 60°C for 2 hours. Finally, 2.69 kg of white or off-white needle crystals were obtained.

[0033] The purity o...

Embodiment 3

[0035] Dissolve 14kg of naringin in 48kg of methanol and stir for 30 minutes at room temperature. Cool down to 0°C, add a certain amount of concentrated acetic acid dropwise, adjust the pH value to 4.0, and control the temperature at 0-15°C during the dropwise addition.

[0036] After the dropwise addition, the temperature was gradually raised to 73° C., and the reaction was stirred for 40 hours.

[0037] Methanol was removed under reduced pressure to obtain crude naringenin.

[0038] Add 57kg of anhydrous methanol to the obtained crude naringenin, heat to 52°C, and dissolve until clear. Add 560 grams of activated charcoal; stir for 1 hour.

[0039] Filter off activated carbon, then add 58kg of purified water, cool to room temperature and crystallize for 48 hours.

[0040] Suction filtration, rinse the filter cake with an appropriate amount of anhydrous methanol, and dry in a vacuum oven at 60°C for 2 hours. Finally, 3.73 kg of white or off-white needle crystals were obtai...

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PUM

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Abstract

The invention provides a preparation method of naringenin. The preparation method comprises the following steps: (1) preparing solution of naringin in lower alcohol or lower ketone solvent, leading the naringin in the prepared solution to be subjected to acid hydrolysis in an acidic condition to obtain naringenin, distilling under reduced pressure to remove solvent to obtain a naringenin crude product; (2) dissolving the naringenin crude product in absolute ethanol or absolute methanol, adding active carbon, stirring to decolor; and (3) filtering the active carbon, separating and purifying the prepared solution to obtain the naringenin. The preparation method has the advantages of few reaction steps, less used solvent, less emission of the 'three wastes', mild reaction condition and complete reaction and easy operation, is suitable for industrial production, and has higher practical value; and the prepared product has more stable quality, the purity is higher than 99 percent, which is higher than the drug standard.

Description

technical field [0001] The present invention generally relates to a method for preparing naringenin, in particular to a method for preparing high-purity naringenin by hydrolyzing naringenin. Background technique [0002] Naringenin is the aglycone of naringin, also known as citrusin, naringenin, naringenin, citrusin, and is a dihydroflavonoid compound that exists in a variety of plants; it can be extracted from a variety of plants, It can also be obtained from the hydrolysis of naringin. Naringenin has antibacterial, anti-inflammatory, anti-tumor, free radical scavenging, antispasmodic and choleretic effects. Since the content of naringenin in natural plants is not high, complex extraction and separation processes are required, the discharge of three wastes is large and it is not easy to recycle; while naringin is relatively high in content and easy to extract. [0003] Liu Yaping disclosed a preparation method of naringenin in "Research on the preparation method of naring...

Claims

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Application Information

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IPC IPC(8): C07D311/32C07D311/40
Inventor 樊振吕和平张向飞吴总社王卫王辉邵曙光焦国华任清华吴相永吕兰亭孔德周臧文生孟利沙
Owner HENAN TOPFOND PHARMA
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