Carbon Dioxide → HCID 13127600, compound

Participants

Reaction Steps

Sodium (0.5 g) was added to a stirred mixture of 4-cyano-5-di(phenoxycarbonyl)amino-1-(2,3,4-trichlorophenyl)pyrazole (prepared as described in Example 27; 25 g) in t-butanol (400 ml) and the mixture was heated at reflux for 15 minutes. Solid carbon dioxide pellets were then added to the cooled reaction mixture to adjust the pH to 7. The neutralized reaction mixture was filtered and the filtrate evaporated under reduced pressure to give an oil which was crystallised from ethyl acetate-n-hexane to give 5-t-butoxycarbonylamino-4-cyano-1-(2,3,4-trichlorophenyl)pyrazole (11.0 g), m.p. 140°-141° C., in the form of colourless crystals.

Provenance & Evidence