Ammonium Hydroxide → HCID 178434626, compound

Participants

Reaction Steps

Ethyl 3-methyl-4-nitropyrazole-5-carboxylate (82.5 g, 0.41 mol) was heated at reflux in 600 ml of concentrated ammonium hydroxide for 2 hours. Concentrated ammonium hydroxide (100 ml) was added and the solution was heated at reflux for an additional three hours. The solution was concentrated in vacuo until the product began to crystallize. The crude material was recrystallized from 700 ml of water to give 47 g product, m.p. 218°-220° (decomp). From the mother liquor was recovered 25 g of 3-methyl-7-nitropyrazole-5-carboxylic acid. Based on the amount of nitro acid consumed, the yield was 95.8%.

Provenance & Evidence