反应详情

温度

100 °C

A mixture of 25.4 g (0.1 mol) of 96.17% pure 5-chloro-1-phenyl-1H-pyrazole-4-carboxylic acid, ethyl ester, 9.8 g (0.2 mol) of sodium cyanide and 75 ml of DMF was heated at 100° C. for 6 hours. The mixture was cooled and stirred for 17 hours at room temperature. A solution of 27.13 g (0.35 mol) of 40% aqueous methylamine was added dropwise to the reaction mixture over a 5 minute period, and the resulting mixture was stirred at room temperature for 22 hours. Seventy-five milliliters of water were added and the reaction mixture was stirred at room temperature for approximately 1 hour. The precipitate was collected by filtration and vacuum dried to afford 19.4 g of 5-cyano-1-phenyl-N-methy-1H-pyrazole-4-carboxamide. Purity of this material as determined by high pressure liquid chromatography was 98.5%. The corrected yield of the product was 87.9%.

1. temperatureThe mixture was cooled
2. stirringthe resulting mixture was stirred at room temperature for 22 hours
3. stirringthe reaction mixture was stirred at room temperature for approximately 1 hour
4. filtrationThe precipitate was collected by filtration and vacuum
5. customdried