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Method for preparing scutellarin aglycone

A technology of scutellarin aglycon and scutellarin, which is applied in the field of compound preparation, can solve the problems of low solubility of scutellarin and limitation of yield of scutellarin aglycone, and achieve high yield, high purity and high efficiency Effect

Inactive Publication Date: 2010-09-08
NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese invention patent CN 1683357A discloses a method for preparing scutellarin aglycon. However, due to the relatively low solubility of scutellarin in aqueous solution, the yield of scutellarin aglycone is limited

Method used

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  • Method for preparing scutellarin aglycone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation of embodiment 1 scutellarin aglycon

[0031] (1) Get concentrated hydrochloric acid, join concentration and be configured into the concentrated hydrochloric acid ethanol solution that molar concentration is 4mol / L in 95% ethanol, standby;

[0032] (2) Add scutellarin to the alcoholic hydrochloric acid solution prepared in step (1), so that the concentration of scutellarin in the alcoholic hydrochloric acid solution is 0.05g / ml, and then reflux reaction at 80°C under nitrogen protection for 5 hours, and the reaction while stirring;

[0033] (3) After the reaction is over, take the reaction solution and evaporate half of the volume of ethanol, then add ice water with 5 times the volume of the reaction solution, cool and crystallize, suction filter after the crystallization is complete, get the solid and recrystallize it with ethyl acetate to obtain After crystallization, recrystallize with 80% methanol solution to obtain scutellarin aglycone with a yield ...

Embodiment 2

[0034] The preparation of embodiment 2 scutellarin aglycon

[0035] (1) Get concentrated hydrochloric acid, join concentration and be configured into the concentrated hydrochloric acid ethanol solution that molar concentration is 6mol / L in 95% ethanol, standby;

[0036] (2) Add scutellarin to the alcoholic hydrochloric acid solution prepared in step (1), so that the concentration of scutellarin in the alcoholic hydrochloric acid solution is 0.05g / ml, and then reflux reaction at 85°C under nitrogen protection for 5 hours, the reaction while stirring;

[0037] (3) After the reaction is over, take the reaction solution and evaporate half the volume of ethanol, then add 5 times the volume of ice water to the reaction solution, cool and crystallize, suction filter after the crystallization is complete, get the solid and recrystallize it with acetone to obtain the crystallized Then recrystallize with 80% ethanol solution to obtain scutellarin aglycone with a yield of 93% and a purity...

Embodiment 3

[0038] Example 3 Preparation of scutellarin aglycone

[0039] (1) Get concentrated hydrochloric acid, join concentration and be configured in the concentrated hydrochloric acid ethanol solution that molar concentration is 8mol / L in 95% ethanol, standby;

[0040] (2) Add scutellarin to the alcoholic hydrochloric acid solution prepared in step (1), so that the concentration of scutellarin in the alcoholic hydrochloric acid solution is 0.08g / ml, and then reflux reaction at 90°C under nitrogen protection for 4 hours, the reaction while stirring;

[0041] (3) After the reaction is over, take the reaction solution and evaporate half of the volume of ethanol, then add ice water with 5 times the volume of the reaction solution, cool and crystallize, suction filter after the crystallization is complete, get the solid and recrystallize it with ethyl acetate to obtain After crystallization, recrystallize with 90% ethanol solution to obtain scutellarin aglycone with a yield of 88%, and i...

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Abstract

The invention discloses a method for preparing scutellarin aglycone. In the method, 95 percent ethanol is used as reaction solution; and scutellarin undergoes hydrolysis reaction in 3 to 8 mol / L organic acid alcohol solution under the protection of an inert gas to prepare high-purity scutellarin aglycone. Due to the adoption of the method for preparing the scutellarin aglycone provided by the invention, an optimal preparation process for the scutellarin aglycone is determined; the overall preparation method has the characteristics of fast reaction speed and high efficiency; the obtained scutellarin aglycone has the characteristics of high yield and high purity; and the method for preparing the scutellarin aglycone provided by the invention has high operability and can realize industrialized mass production.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a method for preparing scutellarin aglycone by acid hydrolysis using flavonoid compound scutellarin as a raw material. Background technique [0002] Scutellarin aglycon is a flavonoid compound in breviscapus breviscapus, a plant of the family Asteraceae. Erigeron breviscapus is cold in nature, slightly bitter, sweet and warm, and has the effects of dispelling cold and relieving the exterior, expelling wind and dampness, promoting blood circulation and removing blood stasis, dredging meridian and activating collaterals, reducing inflammation and relieving pain. Scutellarin is a flavonoid active ingredient extracted from the natural plant scutellaria breviscapus, including a mixture of scutellarin and scutellarin, mainly scutellarin (the content accounts for more than 95%). Breviscapine preparations have been used clinically since the 1970s. Through nearly 30 years of clinical...

Claims

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Application Information

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IPC IPC(8): C07D311/30
Inventor 李念光唐于平段金廒
Owner NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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