Medicine for preventing and treating osteoporosis and preparation method thereof
A technology of derivatives and flavonoids, applied in the field of natural medicine, can solve problems such as reduced effect
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Embodiment 1
[0049] Embodiment 1: the preparation of compound Y-1:
[0050]
[0051] Step (1): Dissolve (1.379g, 8.2mmol) substituted acetophenone F-1 and (0.536g, 4mmol) m-phthalaldehyde in 10mL propanol, add sodium hydroxide dropwise under nitrogen protection and ice-water bath The solution (7.2 g dissolved in 8 mL water) was heated to 75° C. and kept at this temperature for 10 hours. Add 10% hydrochloric acid to neutralize to about pH 7, extract with dichloromethane, and then separate and purify by silica gel column chromatography (eluent: ethyl acetate:petroleum ether (60-90°C)=20:1) to obtain 1.01g Chalcone M-1, the yield is 58%;
[0052] Step (2): Dissolve (0.87g, 2mmol) chalcone M-1 in dimethyl sulfoxide, add 4 drops of concentrated sulfuric acid, heat up to 100°C and stir for 10min, then add 12.8mg (0.05mmol) iodine, Continue to react at a temperature of 100°C for 16 hours, after cooling, add 20mL of water, extract with ethyl acetate, then use silica gel column chromatography ...
Embodiment 2
[0053] Embodiment 2: the preparation of compound Y-2:
[0054]
[0055] Step (1): Dissolve (1.64g, 9.0mmol) substituted acetophenone F-2 and (0.536g, 4mmol) isophthalaldehyde in 10mL of acetonitrile, and add potassium hydroxide solution dropwise under nitrogen protection and ice-water bath (8.8 g dissolved in 8 mL of water), the temperature was raised to 80° C., and the reaction was maintained at this temperature for 12 hours. Add 10% hydrochloric acid to neutralize to about pH 7, extract with dichloromethane, and then use silica gel column chromatography (eluent is dichloromethane:methanol=5:2) to separate and purify to obtain 1.165g of chalcone M-2, The yield is 63%;
[0056] Step (2): Dissolve (0.925g, 2mmol) chalcone M-2 in DMF, add 5 drops of concentrated sulfuric acid, heat up to 100°C and stir for 15min, then add 15.4mg (0.06mmol) iodine, at 100°C The reaction was continued for 24 hours at a certain temperature, and after cooling, 25 mL of water was added, extracte...
Embodiment 3
[0057] Embodiment 3: the preparation of compound Y-3:
[0058]
[0059] Step (1): Dissolve (1.28g, 7.0mmol) substituted acetophenone F-3 and (0.40g, 3mmol) m-phthalaldehyde in 10mL ethanol, and add potassium carbonate solution dropwise under nitrogen protection and ice-water bath ( 9.2g was dissolved in 10mL water), the temperature was raised to 75°C, and the reaction was kept at this temperature for 10 hours. Add 20% sulfuric acid to neutralize to about pH 7, extract with dichloromethane, and then use silica gel column chromatography (eluent is dichloromethane:ethanol=3:1) to separate and purify to obtain 0.60g chalcone M-3, The yield is 43%;
[0060] Step (2): Dissolve (0.46g, 1mmol) chalcone M-3 in dimethyl sulfoxide, add 4 drops of concentrated sulfuric acid, heat up to 100°C and stir for 10min, then add 6.4mg (0.025mmol) iodine, Continue to react at a temperature of 100° C. for 22 hours, after cooling, add 20 mL of water, extract with ethyl acetate, then separate and...
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