Pentachloropyridine → HCID 21331926, compound

Participants

Reaction Conditions

Reaction Steps

Sodium hydride (4.8 grams of 57% oil dispersion) was washed with pentane and 30 ml. of DMF was added under nitrogen. The slurry was stirred and cooled to 0° C. To this was added a solution of 4-nitro-2-trifluoromethylaniline (11.0 grams, 0.053 mole) in 20 ml. of DMF; the addition was carried out slowly, keeping the temperature of the reaction mixture below 10° C. The reaction mixture was stirred for one hour, slowly reaching room temperature. The reaction mixture was then cooled to 0° C., pentachloropyridine (10 grams; 0.059 mole) added, and the reaction mixture stirred for 72 hours, slowly reaching room temperature. A yellow solid crystallized. It was separated and recrystallized from ethanol. Elemental analysis showed:

Provenance & Evidence