反应详情

18.8 g of 1-methylpyrazole-5-carboxylic acid (mp 227° to 228° C.) are stirred in a mixture consisting of 23.5 of 100% strength nitric acid and 17 ml of 25% strength oleum for 8 hours at from 55° to 60° C. and for 4.5 hours at from 70° to 75° C. The mixture is poured onto ice and extracted with 9:1 methylene chloride/ethanol. The extract is concentrated. This yields 27 g of 1-methyl-4-nitropyrazole-5-carboxylic acid, mp 162° to 164° C., with decomposition (from ethyl acetate).

1. additionThe mixture is poured onto ice
2. extractionextracted with 9:1 methylene chloride/ethanol
3. concentrationThe extract is concentrated