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Method for preparing protopanoxadiol and protopanaxatriol by using synergistic oxidation and alkaline bydrolysis of oxide and hyperoxide

A technology of protopanaxadiol and protopanaxatriol, which is applied in the fields of steroids and organic chemistry, can solve the problems of sodium alkoxide, such as easy water absorption failure, difficult storage and transportation, and affecting hydrolysis yield, etc., and achieves short reaction time and high raw material The effect of abundant sources and shortened reaction time

Active Publication Date: 2010-01-27
中山以诺生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The alkali used in this method is sodium alkoxide, a large amount of heat is wasted in the process of producing sodium alkoxide, and sodium alkoxide is easy to absorb water and fail, storage and transportation are difficult, which affects the hydrolysis yield. In addition, this method also has the disadvantage of long reaction time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0026] In a 2L four-necked bottle equipped with a thermometer, an oxygen inlet tube, and a sealed rubber tube on the top (the other end of the rubber tube is connected to a funnel, which is immersed in a beaker filled with liquid paraffin), a 2L four-necked bottle is added. gram and 1300ml of n-propanol, after stirring for 10 minutes, add 40 grams of sodium metal, and when no hydrogen gas is released, add 10 grams of benzoyl peroxide, start oxygen flow, and heat the reaction solution to 86 ° C for 24 hours. After the reaction, the reaction liquid was cooled to room temperature, washed with water three times, the n-propanol layer was vacuum-dried and dissolved in water, first extracted with n-hexane with low polarity substances, then extracted with ethyl acetate, evaporated to dry ethyl acetate to obtain the original Panaxadiol and protopanaxatriol mixture crude product, crude product is through silica column chromatography, adopts 1~5% methanol / chloroform solution gradient wash...

example 2

[0028] In a 2L four-necked bottle equipped with a thermometer, an oxygen inlet tube, and a sealed rubber tube on the top (the other end of the rubber tube is connected to a funnel, which is immersed in a beaker filled with liquid paraffin), a 2L four-necked bottle is added. gram and 1300ml of n-butanol, after stirring for 10 minutes, add 40 grams of sodium metal, and react until no hydrogen is released, add 10 grams of benzoyl peroxide, start oxygen flow, and heat the reaction solution to 90 ° C for 24 hours. After the reaction, the reaction solution was cooled to room temperature, washed with water three times, the n-butanol layer was vacuum-dried and dissolved in water, first extracted with n-hexane with low polarity substances, then extracted with ethyl acetate, evaporated to dry ethyl acetate to obtain the original Panaxadiol and protopanaxatriol mixture crude product, crude product is through silica column chromatography, adopts 1~5% methanol / chloroform solution gradient w...

example 3

[0031]In a 2L four-necked bottle equipped with a thermometer, an oxygen inlet tube, and a sealed rubber tube on the top (the other end of the rubber tube is connected to a funnel, which is immersed in a beaker filled with liquid paraffin), a 2L four-necked bottle is added. gram and 1300ml n-butanol, after stirring for 10 minutes, add 40 grams of sodium metal, and react until no hydrogen gas is released, add 10 grams of benzoyl peroxide, start oxygen flow, and heat the reaction solution to 90 ° C for 48 hours. After the reaction, the reaction solution was cooled to room temperature, washed with water three times, the n-butanol layer was vacuum-dried and dissolved in water, first extracted with n-hexane with low polarity, then extracted with ethyl acetate, evaporated to dryness of ethyl acetate to obtain the original Panaxadiol and protopanaxatriol mixture crude product, crude product is through silica column chromatography, adopts 1~5% methanol / chloroform solution gradient washi...

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Abstract

This invention relates to a method for preparing protopanaxadiol and protopanaxatriol by co-oxidizing with oxygen and peroxide and alkali-hydrolyzing total notoginsenoside. The method comprises: (1) oxidizing and alkali-hydrolyzing Panax ginseng total saponin extract and Gynostemma pentaphyllum total saponin extract by applying cooperative effect of oxygen and peroxide, and alkali-hydrolyzing using alkoxide in situ formed in alcohol at 80-95 swg..C for 8-24 h, where the Panax ginseng total saponin extract and Gynostemma pentaphyllum total saponin extract / alcohol ratio is 30-150 g / L; (2) purifying by column chromatography to obtain protopanaxadiol and protopanaxatriol. The method adopts cooperative effect of oxygen and peroxide, thus can obtain high-purity protopanaxadiol and protopanaxatriol with high yields at low reaction temperatures and short reaction time. This invention provides a simple, convenient and low-cost method for preparing protopanaxadiol and protopanaxatriol in large amounts, which can satisfy the needs of drugs for treating cardiovascular and cerebrovascular diseases and tumor.

Description

【Technical field】 [0001] The present invention relates to a method for preparing protopanaxadiol and protopanaxatriol from the total saponins extract of plants of the genus Panax and the total saponins extract of Gynostemma pentaphyllum of Cucurbitaceae plants, in particular, under the synergistic action of oxygen and peroxide, through alcohol and The invention relates to a preparation method of strong alkali hydrolysis in which alkali metal is generated in situ in alcohol. 【Background technique】 [0002] Ginseng is a perennial herb belonging to the Araliaceae Panax genus. Ginseng mainly contains saponins, namely ginsenosides, sugars, volatile oils, fatty oils, sterols, amino acids, vitamins and other substances, among which ginsenosides are the main components of ginseng. Ginsenosides currently separated and refined through scientific and advanced technology are named Ro, Ra1, Ra2, Rb1, Rb2, Rb3, Rc, Rd, Rf, Rg1, Rg2, Rg3, Rh1, Rh2, I, K, O-glaco is composed of aglycone a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00
Inventor 曹德榕徐社阳余佩华邓跃敏
Owner 中山以诺生物科技有限公司
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