Hedera saponin derivatives and their application in the preparation of drugs for preventing and treating senile dementia
A technology of helexin and senile dementia, which can be used in drug combinations, steroids, organic chemistry, etc., and can solve problems such as reports that no application has been found.
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example 1
[0052] Preparation of (3β,4a)-3,23-dihydroxyolean-12-en-28-acid (compound Ⅰ, hedera saponin)
[0053] Take 1 kg of Dipsacus medicinal material, and reflux extract with 8 times the amount of 75% ethanol for 3 times. For 3 hours each time, combine three extracts, add 30g of calcium oxide, stir, stand overnight, filter, adjust the pH of the filtrate to 6-7 with dilute hydrochloric acid, add 200g of activated carbon, stir, filter, and recover ethanol from the filtrate until it is free of alcohol Add water to 2000ml, pass through the treated macroporous resin column, first wash 3 times the column volume with 20% ethanol with a pH value of 12, then wash with water until neutral, finally elute with 70% ethanol, collect 70% The eluate was concentrated to dryness under reduced pressure; hydrolyzed with 12 times the amount of 2N hydrochloric acid and 40% ethanol for 3 hours. Filtrate, discard the hydrolyzate, wash the filter cake with deionized water until neutral; then heat to boiling...
example 2
[0055] Preparation of (3β,4a)-3,23-diacetyl-olean-12-ene-28-acid (compound Ⅱ):
[0056] Take 10mmol of compound N1 (RA, 4.72g), add 200mL of pyridine, 100mL of acetic anhydride, react at 80°C, and detect the end point of the reaction by TLC. After the reaction is completed, recover the solvent under reduced pressure, add water to 250mL, and adjust the pH to 5 with dilute hydrochloric acid. , filtered, the filter cake was washed with water until colorless, dissolved in 250 mL of ethyl acetate, washed twice with water, 100 mL each time, washed three times with 10% sodium carbonate, 100 mL each time, and then washed with 100 mL of 1mol / L hydrochloric acid Wash once, and finally wash twice with water, 100 mL each time, recover ethyl acetate to dryness, add 300 mL of ethanol for recrystallization, and dry to obtain compound II (3.88 g). Yield 69.9%. White powder; mp 298~299℃; IR(KBr)ν max :3 597,3 443,2 955,2 873,1 727,1 704,1 472,1 370,1 036,924cm -1 ; HR-ESI-MS m / z: 557.380 4 ...
example 3
[0058] Preparation of 2-[(3β,4a)-3,23-diacetyl-olean-12-en-28-yl]-aminoethanol (compound Ⅲ)
[0059] Take 1.3mmol of compound N2 (0.723g), dissolve it in 15mL of dichloromethane, add 1.2mL of oxalyl chloride, react in ice bath for 1h, then react at room temperature, and detect the end point of the reaction by TLC. After the reaction is completed, concentrate under reduced pressure at 30°C to dry. Add dichloromethane to recover under reduced pressure, repeat 3 times, 50mL each time, dissolve with 8mL of dichloromethane, adjust the pH to 9-10 with triethylamine, add 0.8mL of ethanolamine, react at room temperature for 1.5h, add 50mL of water, dissolve with dilute hydrochloric acid Adjust the pH to 3-4, recover the solvent, filter, recrystallize the filter residue with 300mL of ethanol, dry, separate by silica gel column chromatography, and wash with petroleum ether (60-90°C)-ethyl acetate (1:3) as developing solvent Removed, combined the same components, recovered the solvent, ...
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