Hydrochloric Acid → HCID 22769692, compound

Participants

Reaction Conditions

Reaction Steps

2,6-dichloroaniline (360 g.) was dissolved in dimethylformamide (1.5 l.) and added to sodium hydride (obtained by washing sodium hydride in mineral oil (214 g; 50%) with petrol) suspended in dimethylformamide (4.1) at 10° C. When the addition was completed the temperature of the mixture was allowed to rise to the ambient temperature and then cooled to 10° C. A solution of 2-chloro-3,5-dinitrobenzotrifluoride (600 g.) in dimethylformamide (1.5 l.) was slowly added, and the mixture stirred at the ambient temperature for 20 hours. The mixture was poured into salt/iced water (20.1) and the resultant mixture acidified with concentrated hydrochoric acid. The precipitate was collected by decanting off the supernatant liqui and recrystallised from methylated spirit to yield 2(2,6-dichloroanilino)-3,5-dinitrobenzotrifluoride, melting point 97°-99° C.

Provenance & Evidence