Method for preparing veratric acid from trollius chinensis bunge

A technology of nasturtium and veratronic acid, applied in the field of preparation of veratronic acid, can solve the problems of unreported yield and cumbersome steps

Inactive Publication Date: 2011-02-02
BEIJING UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method can obtain veratrol, the steps are cumbersome, including degreasing, ethanol extraction, sodium carbonate solution treatment, pH adjustment, repeated extraction with ether, activated carbon decolorization, repeated recrystallization and pH adjustment, etc., and the author did not report the yield.

Method used

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  • Method for preparing veratric acid from trollius chinensis bunge

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Effect test

Embodiment 1

[0012] Take 10g of nasturtium herb, add 15 times the amount (v / w) of ethyl acetate, reflux extraction in a 90°C water bath for 2h, concentrate the extract to 20ml, add 10g of polyamide powder to mix the sample. After the mixture was evaporated to dryness under reduced pressure, it was put into a Buchner funnel, and 200ml of 20% ethanol was added to filter it with suction. After the filtrate was concentrated to dryness, repeated recrystallization with petroleum ether-acetone gave 23 mg of veratronic acid with a purity of 98.2%.

Embodiment 2

[0014] Take 10g of nasturtium herb, add 10 times the amount (v / w) of ethyl acetate, reflux extraction on a 90°C water bath for 2h, concentrate the extract to 20ml, add 10g of polyamide to mix the sample. After the mixture was evaporated to dryness under reduced pressure, it was put into a Buchner funnel, and 200ml of 20% ethanol was added to filter it with suction. After the filtrate was concentrated to dryness, repeated recrystallization with petroleum ether-acetone gave 18 mg of veratronic acid with a purity of 98.5%.

Embodiment 3

[0016] Take 10 g of nasturtium herb, add 20 times the amount (v / w) of ethyl acetate, reflux extraction on a 90°C water bath for 2 hours, concentrate the extract to 20 ml, add 10 g of polyamide to mix the sample. After the mixture was evaporated to dryness under reduced pressure, it was put into a Buchner funnel, and 200ml of 20% ethanol was added to filter it with suction. After the filtrate was concentrated to dryness, repeated recrystallization with petroleum ether-acetone gave 25 mg of veratronic acid with a purity of 97.9%.

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Abstract

The invention relates to a method for preparing veratric acid from trollius chinensis bunge. The method comprises the following steps: adopting 15 times amount of ethyl acetate to carry out direct reflux extraction on the trollius chinensis bunge twice, 2h each time, concentrating the extracts to certain volume and uniformly mixing the concentrated extracts with powdered polyamide with weight doubling that of the drug, drying the mixture, carrying out suction filtration on the solid particle mixture with 20 times amount of 20% of ethanol and recrystallizing the concentrated suction filtrate with petroleum ether-acetone to obtain the veratric acid.

Description

field of invention [0001] The invention relates to a method for preparing veratrol from nasturtium. Background technique [0002] Veratronic acid (3,4-dimethoxybenzoic acid) is a commonly used chemical synthesis intermediate, widely used in industry, medicine, agriculture and other fields, and is a key intermediate for the synthesis of drugs such as alfuzosin hydrochloride . At present, the preparation of veratrol is mainly based on chemical synthesis, and the commonly used synthetic methods mainly include: (1) in the organic solvent tert-butanol, take reveratrol as raw material, add 1,3-dinitrobenzene and tert-butanol Potassium, oxygen as an oxidant, synthesizes the target compound (Hans-René et al. Tetrahedron Letters, 2002, 43(28): 4985-4987). Potassium tert-butoxide and reveratrol used in the synthesis method are expensive, and the synthesis cost is relatively high. (2) Using veratraldehyde as the main raw material, disproportionate it with aldehyde and alkali to fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/21C07C51/42
Inventor 王如峰孙震晓张彤
Owner BEIJING UNIV OF CHINESE MEDICINE
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