Nitric Acid → HCID 19993698, compound

Participants

Reaction Steps

Fuming nitric acid (5 ml) was added to an ice-cooled solution of 3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-difluoromethoxypyrazole (1.5g) in concentrated sulfuric acid (20 ml). The mixture was stirred at room temperature for 3 hours then poured into ice/water and extracted into dichloromethane (3×50 ml). The combined dichloromethane extracts were washed with water (30 ml), filtered through phase-separation paper and evaporated in vacuo. The resultant gum was purified by dry-column chromatography (eluant ether:hexane 1:3) t give 3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-difluoromethoxy-5-nitropyrazole (0.3g) as a yellow solid, m.p. 72.5°-74° C.

Provenance & Evidence