反应详情

温度

70 °C

A mixture of 1-methyl-5-(2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamoyl)-1H-pyrazole-4-carboxylic acid (100 mg, 276 μmol), thiomorpholine-1,1-dioxide (44.8 mg, 331 μmol), diisopropylethylamine (145 μl, 828 μmol) and propylphosphonic anhydride (50% in ethyl acetate, 407 μl, 690 μmol) in tetrahydrofurane (7.00 ml) is stirred for 4 hours at 70° C. and then for 60 hours at 25° C. under nitrogen atmosphere. The solvent is evaporated and to the residue is added sat. aqueous sodium hydrogencarbonate solution. The mixture is stirred for 20 minutes while a white solid precipitates. The solid is collected by filtration, washed with diethylether and dried affording 4-(1,1-dioxo-thiomorpholine-4-carbonyl)-2-methyl-2H-pyrazole-3-carboxylic acid (2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-yl)-amide (112 mg, 84.7%) as a white solid. mp.: >250° C. MS: m/z=480.2 (M+H+).

1. waitfor 60 hours at 25° C. under nitrogen atmosphere
2. customThe solvent is evaporated and to the residue
3. additionis added sat. aqueous sodium hydrogencarbonate solution
4. stirringThe mixture is stirred for 20 minutes while a white solid
5. customprecipitates
6. filtrationThe solid is collected by filtration
7. washwashed with diethylether
8. customdried