Bromoform → HCID 13689612, compound

Participants

Reaction Steps

18 ml (0.16 mole) of t-butyl nitrite are added dropwise to 17.1 g (0.05 mole) of 5-amino-4-nitro-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole (compare DE-OS (German Published Specification) No. 3,402,308), supra, in 75 ml of bromoform in the course of 15 minutes, with stirring, whereupon the temperature of the reaction mixture rises to 50° C. When the addition has ended, the mixture is stirred at the reflux temperature for a further hour and concentrated in vacuo. 18.0 g (89% of theory) of 1-(2,6-dichloro-4-trifluoromethyl-phenyl)-4-nitro-5-bromo-pyrazole of melting point 96° C. are obtained.

Provenance & Evidence