Hydrochloric Acid → HCID 21188104, compound

Participants

Reaction Steps

To a stirred solution of 5-chloro-3-cyano-)-4-(2,2-dibromoethenyl)-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole (2.12 g) in dimethylsulphoxide (8 ml) at 15° C. was added dropwise a solution of 1,8-diazabicyclo[5.4.0]undec-7-ene (1.21 ml) in dimethylsulphoxide (7.9 ml). After two hours the reaction mixture was neutralism with 0.5N hydrochloric acid and partitioned between water and dichloromethane. The aqueous layer was thrice extracted with dichloromethane. The combined organic layers were washed with brine, dried (Na2SO4) and evaporated. The aqueous layer was thrice extracted with dichloromethane. The combined organic layers were washed with brine, dried (Na2SO4) and evaporated. The residue was purified by column chromatography on silica gel eluted with hexane dichloromethane (1:1). Combination and evaporation of suitable fractions followed by recrystallisation from hexane gave the title compound as a light pink solid, m.p. 109.1-109.9° C.

Provenance & Evidence