2-pyridine derivatives as inhibitors of neutrophile elastase
A compound, C1-C6 technology, used in non-central analgesics, drug combinations, organic active ingredients, etc., can solve problems such as tissue destruction
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Embodiment 1
[0268] N-{[3-(2-Hydroxyethyl)isoxazol-5-yl]methyl}-6-methyl-5-(1-methyl-1H-pyrazole-5- Base)-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxamide
[0269] a) 5-iodo-6-methyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2-dihydro-pyridine-3-carboxylic acid prop-2-ynylamide
[0270] In a flask, 6-methyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2-dihydro-pyridine-3-carboxylic acid (as described in Intermediate Example 1 Prepared as described above, 0.5g, 1.68mmol) was dissolved in CH 2 Cl 2 (7ml) and TFA (3ml). N-iodosuccinimide (0.378 g, 1.68 mmol) was added, and the mixture was stirred at room temperature for 1 hour. Volatiles were removed by evaporation to give the 5-iodinated product, which was dissolved in CH 2 Cl 2 (5ml), add SOCl 2 (5ml). The mixture was stirred for 1 hour, then concentrated well. The crude solid acid chloride was dissolved in 1,4-dioxane (10ml, anhydrous) and a mixture of Hunigs base (DIPEA, 1ml) and propargylamine (0.165g, 3mmol) was add...
Embodiment 2
[0280] 5-(3,5-Dimethylisoxazol-4-yl)-N-{[3-(2-hydroxyethyl)isoxazol-5-yl]methyl}-6-methanol Base-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2-dioxypyridine-3-carboxamide
[0281] According to the method described in Example 1c, from 5-iodo-6-methyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2-dihydro-pyridine-3-carboxylic acid {3-[2-(Tetrahydro-pyran-2-yloxy)-ethyl]-isoxazol-5-ylmethyl}-amide (Example 1b, 0.032g, 0.051mmol), 3, 5-Dimethylisoxazol-4-yl-boronic acid (0.020g, 0.142mmol) and Na 2 CO 3 (2M, 1.5ml) The compound was prepared except that the intermediate was partitioned between EtOAc / water and the organic phase was purified on silica followed by hydrolysis. Purification by preparative HPLC and lyophilization afforded 0.010 g (38%) of the title compound as a white solid.
[0282] 1 H NMR (DMSO-d 6 ): δ9.88(1H, t, J=6.3Hz); 8.18(1H, s); 8.01(1H, d, J5.5Hz); 7.92(1H, d, J 7.2Hz); 7.87-7.79(2H , m); 6.23(1H, s); 4.60(2H, d, J6.3Hz); 3.62(2H, t, J 6.6Hz); 2.69(2H, t, J 6.6H...
Embodiment 3
[0285] N-{[3-(2-Hydroxyethyl)isoxazol-5-yl]methyl}-5-iodo-6-methyl-2-oxo-1-[3-(trifluoromethyl Base) phenyl] -1,2-dihydropyridine-3-carboxamide
[0286]Hydrolysis of 5-iodo-6-methyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2-dihydro-pyridine-3-carboxylic acid according to the hydrolysis procedure described in Example 1c {3-[2-(Tetrahydro-pyran-2-yloxy)-ethyl]-isoxazol-5-ylmethyl}-amide (Example 1b, 0.14g, 0.22mmol). Purification by preparative HPLC and lyophilization afforded 0.060 g (50%) of the title compound as a white solid.
[0287] Intermediate Example 2
[0288] 6-methyl-5-(2-methyl-2H-pyrazol-3-yl)-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2-dihydro- Pyridine-3-carboxylic acid
[0289] a) 6-methyl-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylic acid ethyl ester
[0290] Under nitrogen atmosphere, 6-methyl-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylic acid (Intermediate Example 1b, 13.1 g, 43.9 mmol), sodium carbonate (5....
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