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
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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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