New piperazine derivative and medical applications
A derivative, piperazine technology, applied in the field of new piperazine derivatives and their medical applications, can solve the problems of limited clinical application and low bioavailability
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Embodiment 1
[0053] Example 1N-(resveratrol-4'-oxycarbonylpropionyl)-piperazine (Ia-1) and N-(resveratrol-3-oxycarbonylpropionyl)-piperazine (Ib-1) preparation of
[0054]
[0055] 1.1 Synthesis of resveratrol-4'-oxycarbonylpropionic acid and resveratrol-3-oxycarbonylpropionic acid
[0056] Add 10g (43.8mmol) of resveratrol to 200ml of dry dichloromethane, add 4.38g (43.8mmol) of succinic anhydride, add 5ml of anhydrous pyridine, and stir at 40°C for 12 hours. It was washed successively with 0.5N hydrochloric acid and saturated aqueous sodium chloride solution, and the organic layer was dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The residue was separated by silica gel column chromatography, eluted with a mixed solvent of ethyl acetate:petroleum ether:acetic acid (2:10:0.2), and the required components were collected respectively, and evaporated to dryness under reduced pressure to obtain resveratrol-4 4.1 g of '-oxycarbonylpropionic acid and ...
Embodiment 2
[0063] Example 2 N-(resveratrol-4'-oxycarbonyl butyryl)-piperazine (Ia-2) and N-(resveratrol-3-oxycarbonyl butyryl)-piperazine (Ib-2) preparation of
[0064]
[0065] 2.1 Synthesis of resveratrol-4′-oxycarbonyl butyric acid and resveratrol-3-oxycarbonyl butyric acid
[0066] Add 10g (43.8mmol) of resveratrol to 200ml of dry dichloromethane, add 5.0g (43.8mmol) of glutaric anhydride, add 5ml of anhydrous pyridine, and stir at 40°C for 12 hours. It was washed successively with 0.5N hydrochloric acid and saturated aqueous sodium chloride solution, and the organic layer was dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The residue was separated by silica gel column chromatography, eluted with a mixed solvent of ethyl acetate:petroleum ether:acetic acid (2:10:0.2), and the required components were collected respectively, and evaporated to dryness under reduced pressure to obtain resveratrol-4 4.0 g of '-oxycarbonyl butyric acid and 1.9 g...
Embodiment 3
[0071] Dissolve 0.56g of N-(resveratrol-3-oxycarbonylbutyryl)-piperazine (Ib-2) with the minimum amount of methanol, drop into the ether solution of hydrogen chloride until no precipitate precipitates; place overnight at 4°C, filter , and dried to obtain 0.3 g of the hydrochloride salt of Ib-2, with a melting point of 97-102° C., and its solubility in distilled water was determined to be 10 mg / ml. Embodiment 3N-(curcumin-4'-oxycarbonyl propionyl)-piperazine (Ic-1)
[0072]
[0073] Add 3.68g (10mmol) of curcumin to 100ml of dry dichloromethane, add 1.0g (10mmol) of succinic anhydride, add 1ml of anhydrous pyridine, and stir at 40°C for 12 hours. It was washed successively with 0.5N hydrochloric acid and saturated aqueous sodium chloride solution, and the organic layer was dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The residue was separated by silica gel column chromatography, eluted with a mixed solvent of ethyl acetate:petroleum ...
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