Echinocystic acid derivative and application thereof in preparation of anti-tumor medicine
A kind of derivative, the technology of echinocystic acid, which is applied in the field of medicine, can solve the problems of no literature report on the growth of echinocystic acid tumor cells, no report on the application of echinocystic acid derivative antitumor drugs, etc.
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example 1
[0026] The preparation of example 1 echinocystic acid
[0027] Take 1 kg of saponin root medicinal material, add 30 g of calcium oxide by weight of the medicinal material, and reflux extract with 8 times the amount of 50% ethanol for 3 times, each time for 2 hours. Combine the extracts three times, filter, and recover the ethanol from the filtrate until it has no alcohol smell, add water to the weight of the medicinal material to 3000ml, pass through the treated macroporous resin column, and first elute with 20% ethanol containing sodium hydroxide (pH value is 13) 3 times the column volume, then eluted with water until neutral, and finally eluted with 70% ethanol for 4 times the column volume, collected the eluate, and concentrated to dryness under reduced pressure; Hydrolyzed for 3 hours. Filtrate, discard the hydrolyzate, wash the filter cake with deionized water until it is neutral; then heat it to boiling with 95% ethanol, add 2% medicinal activated carbon of the volume ...
example 2
[0028] The preparation of example 2 (3,16-dibenzoyl) echinocytic acid (compound 1)
[0029] Echinocysic acid 0.47g, dissolved in 25ml CH 2 Cl 2 2ml of benzoyl chloride was slowly added dropwise in an ice bath, then 2ml of triethylamine was added, and the reaction was stirred at room temperature for 24 hours. After the reaction was complete, the solvent was recovered under reduced pressure and dried to obtain a crude product. The crude product was first recrystallized from dichloromethane-petroleum ether, and then separated and purified by silica gel column (petroleum ether: ethyl acetate = 5:1) to obtain 0.35 g of white powdery crystals.
example 3
[0030] The preparation of example 3 (3,16-two o-methylbenzoyl) echinocytic acid (compound 2)
[0031] Echinocysic acid 0.47g, dissolved in 25ml CH 2 Cl 2 2 ml of o-toluyl chloride was slowly added dropwise in an ice bath, then 2 ml of triethylamine was added, and the reaction was stirred at room temperature for 24 hours. After the reaction was complete, the solvent was recovered under reduced pressure and dried to obtain a crude product. The crude product was first recrystallized from dichloromethane-petroleum ether, and then separated and purified by silica gel column (petroleum ether: ethyl acetate = 5:1) to obtain 0.38 g of white powdery crystals.
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