反应详情

温度

80 °C

Thionyl chloride (3.95 g) and N,N-dimethylformamide (catalytic amounts) were added at room temperature to 5-methyl-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxylic acid (3.0 g) described in Reference Example 8 in toluene (55 ml), and stirred at 80° C. for an hour. The solvent and an excess amount of thionyl chloride were evaporated, tetrahydrofuran (55 ml) was added to the residue, 25% aqueous ammonia (44 ml) was added under ice-cooling and stirred at room temperature for two hours. After the reaction, 1N aqueous solution of sodium hydroxide was added, and the precipitated solid was filtered to give 5-methyl-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxamide (2.9 g) as a white solid.

1. customThe solvent and an excess amount of thionyl chloride were evaporated
2. additiontetrahydrofuran (55 ml) was added to the residue, 25% aqueous ammonia (44 ml)
3. additionwas added under ice-
4. temperaturecooling
5. stirringstirred at room temperature for two hours
6. customAfter the reaction, 1N aqueous solution of sodium hydroxide
7. additionwas added
8. filtrationthe precipitated solid was filtered