反应详情

A mixture of 1-methyl-5-(2-(pyridin-3-yl)-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamoyl)-1H-pyrazole-4-carboxylic acid (100 mg, 223 μmol), morpholine (156 μl, 1.79 mmol), propylphosphonic anhydride (50% in ethyl acetate, 329 μl, 558 μmol) and N,N-diisopropylethylamine (114 μl, 669 μmol) in tetrahydrofurane (7 ml) is refluxed for 18 hours. The mixture is dissolved in ethyl acetate and washed with sodium bicarbonate solution and brine. The organic layer is separated, dried with magnesium sulfate and the solvent is removed under reduced pressure. The residue is purified by chromatography on a 20 g silica column using ethyl acetate/methanol 10% as eluent affording 1-methyl-4-(morpholine-4-carbonyl)-N-(2-(pyridin-3-yl)-[1,2,4]triazolo[1,5-a]pyridin-7-yl)-1H-pyrazole-5-carboxamide (40 mg, 41.5%) as a white solid. mp.: 218-220° C. MS: m/z=433.3 (M+H+).

1. temperatureis refluxed for 18 hours
2. washwashed with sodium bicarbonate solution and brine
3. customThe organic layer is separated
4. dry with materialdried with magnesium sulfate
5. customthe solvent is removed under reduced pressure
6. customThe residue is purified by chromatography on a 20 g silica column