Nitric Acid → HCID 118511093, compound

Participants

Reaction Conditions

Reaction Steps

To trifluoroacetic acid (1940 mL) cooled to −15° C. was added 2-cyclohexyl-1,5-dimethyl-1H-pyrazol-3(2H)-one (535 g, 2231 mmol) and the reaction mixture was allowed to warm to 0° C. Nitric acid 90% (211 mL, 4461 mmol) was added dropwise over 90 minutes maintaining the temperature below 15° C. and the resulting mixture was stirred for 30 minutes at 10° C. The product mixture was slowly poured into ice water (8 L) and stirred for 30 minutes. The solid was collected by filtration and washed with water (2×2 L), saturated sodium bicarbonate solution (1×2 L), water (2×2 L), TBME (3×2 L) and heptane (2×2 L). The solid was dried in the vacuum oven to yield the title compound as a beige powder.

Provenance & Evidence