Application of dimethylamine 4-O-acetyl inula lineariifolia lactone A and salt thereof in preparation of medicine for treating chronic renal failure
A chronic, drug-based technology, applied in the field of medicine, that can solve problems such as shortages
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Embodiment 1
[0036] Example 1 Preparation of Inula Lactone A
[0037] Pulverize 50Kg of dried whole plant of Inula lanceolata, extract 2 times with 750L of 90% ethanol for 2 hours each time, combine the extracts, and concentrate the extracts under reduced pressure into a fluid extract, which is equivalent to 1ml containing the leaves. Inula flower 1.0g, the liquid extract was diluted with 50L of water, and extracted 5 times with 50L of petroleum ether each time to obtain the petroleum ether fraction. The petroleum ether fraction was applied to silica gel column chromatography, eluted with petroleum ether / ethyl acetate system gradient with a volume ratio of 100:0 to 1:1, detected by thin-layer chromatography, and collected. Fraction, and then subjected to C18 reverse-phase column chromatography, eluted with methanol / water with a weight ratio of 50:100-70:100, and detected by thin-layer chromatography to obtain 45.3g of pure inula lactone A. .
[0038] The obtained compound was first measu...
Embodiment 2
[0039] The preparation of embodiment two 4-O-acetyl basal leaf inula lactone A
[0040] Take the above-mentioned inula lactone A (10.0g, 0.027mol, 1.0eq), p-dimethylaminopyridine (DMAP) (4.0g, 0.033mol, 1.2eq) and acetic anhydride (Ac2O) (3.34g, 0.033 mol, 1.2eq) was placed in a 500mL eggplant-shaped flask, 200mL of anhydrous dichloromethane (CH2Cl2) was added, and the mixture was stirred at room temperature for 12h. The reaction was monitored by thin-layer chromatography. After the reaction of the raw materials was completed, 200 mL of water was added to quench, and the water layer was discarded. The organic layer was extracted with 100 mL of water, and the water layer was discarded. Repeat this step until the organic layer No DMAP was detected (TLC method), the organic layer was washed with saturated brine, dried over anhydrous sodium sulfate (Na2SO4), concentrated under reduced pressure below 40°C, and subjected to silica gel column chromatography with a volume ratio of 15:...
Embodiment 3
[0042] The preparation of embodiment three dimethylamine 4-O-acetyl basal leaf inula lactone A
[0043] Take the above-mentioned 4-O-acetyl basal leaf inula lactone A (10.0g, 0.024mol, 1.0eq) and dimethylamine hydrochloride (CH3NHCH3·HCl) (3.0g, 0.037mol, 1.5eq) in 500mL In the eggplant-shaped flask, add 200 mL of ethanol to dissolve, place the reaction flask in a low-temperature cooling tank, and slowly add triethylamine (NEt) dropwise at 0 °C. 3 ) (5.1mL, 0.037mol, 1.5eq), then the reaction system was slowly raised to room temperature (25°C), stirred, and the reaction was monitored by thin layer chromatography. After 4h, the reaction of the raw materials was complete, and the solvent was evaporated under reduced pressure to obtain the crude product , the crude product was dissolved in 200 mL of dichloromethane, and 100 mL of water was added for extraction. The aqueous layer was discarded, and this step was repeated until no dimethylamine hydrochloride was detected in the org...
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