Carbon Tetrachloride → HCID 178526513, compound

Participants

Reaction Steps

A mixture of CF3CO2H (0.98 mL, 12.65 mmol, 0.9 eq), PPh3 (9.21 g, 35.13 mmol, 2.5 eq) and Et3N (1.96 mL, 14.05 mmol, 1.0 eq), in 25 mL CCl4 was stirred at 0° C. for 10 minutes. 2-cyclopropyl-5-nitrobenzeneamine (2.50 g, 14.05 mmol, 1.0 eq) was then added to the reaction mixture and the mixture was heated to reflux for 12 hours. Solvent was removed under reduced pressure and the residue was purified by column chromatography, eluting with n-hexane:ethyl acetate (10:1), giving the (Z)—N-(1-chloro-2,2,2-trifluoroethylidene)-2-cyclopropyl-5-nitrobenzenamine intermediate in semi pure form as a light yellow solid. This compound was taken to the next step with out further purification.

Provenance & Evidence