Halogenated adamantane amide derivatives, preparation method and use thereof
A compound and substituent technology, applied in the field of diabetes-related drugs, can solve problems such as undiscovered weight gain
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Embodiment 1
[0028]
[0029] In a 100mL round bottom flask, add 2.28g (10mmol) compound II-1, 3.21g (10mmol) compound III, 2.06g (10mmol) N, N'-dicyclohexylcarbodiimide (DCC) and 1.22g (10mmol) 4-dimethylaminopyridine (DMAP), dissolved in 20mL of dry THF, stirred at room temperature overnight, TLC showed that the reaction was almost complete. The reaction mixture was suction filtered to remove the solid, the filtrate was evaporated to dryness on a rotary evaporator, and the residue was purified by column chromatography to obtain compound IV-1 as a white solid, ESI-MS, m / z=550 ([M+NH 4 ] + ).
[0030] 3.19 g (6 mmol) of compound IV-1 was dissolved in 30 mL THF, 0.10 g of 10% Pd / C was added, and catalytic hydrogenolysis was carried out at room temperature, and the reaction was completed within 12 hours. The reaction mixture was suction filtered to remove the catalyst, and the filtrate was concentrated on a rotary evaporator, poured into 200 mL of water, stirred, and extracted with 50 mL...
Embodiment 2-4
[0034] Using the same method as in Example 1, the following compounds could be prepared.
[0035]
[0036]
Embodiment 5
[0037] Embodiment 5 compound measures the inhibition of DPP-IV enzyme
[0038] Using the fluorescent DPP4 activity detection kit of BPS Bioscience Company, the inhibitory activity of the compound of the present invention on DPP-IV enzyme was determined.
[0039] Dilute the samples successively according to the concentration of 5, 10, 30, 100 and 200ng / kg, and add the samples in the following table in the fluorescence reaction 96-well plate:
[0040]
[0041] Place in a water bath at 22°C for 10 minutes, use a SpectraMaxM5 type fluorescence detector with an excitation light of 350nm, and measure the absorbance with 450nm fluorescence. Calculation of IC from the concentration-fluorescence intensity curve 50 values, see the table below.
[0042] IC of compounds for inhibition of DPP-IV enzymes 50 value
[0043]
[0044]
[0045] It can be seen from the above table that the compound of the present invention has a strong inhibitory effect on DPP-IV enzyme.
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