反应详情

温度

50 °C

Fuming sulfuric acid (17.8 ml) was added dropwise to stirred, ice-cooled fuming nitric acid (16.0 ml). The resulting solution was heated to 50° C. and 3-n-propyl-1H-pyrazole-5-carboxylic acid (16.4 g, 0.106 mol; Chem. Pharm. Bull., 1984, 32, 1568) added portionwise over 30 minutes whilst maintaining the reaction temperature below 60° C. The resulting solution was heated for 18 hours at 60° C., allowed to cool, then poured onto ice. The white precipitate was filtered, washed with water and dried by suction to yield the title compound as a white solid (15.4 g), m.p. 170-172° C.

1. temperaturewhilst maintaining the reaction temperature below 60° C
2. temperatureThe resulting solution was heated for 18 hours at 60° C.
3. temperatureto cool
4. additionpoured onto ice
5. filtrationThe white precipitate was filtered
6. washwashed with water
7. customdried by suction