Hydrochloric Acid → HCID 21392401, compound

Participants

Reaction Steps

104.4 G. of 3-(1,2-difluoro-1,2,2-trichloroethyl)-nitrobenzene is added over 10 min. to a solution of 325 g. of crystalline stannous chloride (SnCl2 . 2H2O) in 325 g. of concentrated HCl and 325 g. of ethanol with vigorous stirring, maintaining the temperature at 50° C. Stirring is continued for 3 additional hours. It is cooled in ice, and the precipitate collected by filtration. The solids are then suspended in 500 ml. water and 500 ml. of CH2Cl2, the mixture is cooled in ice and made basic by the addition of 50% aqueous NaOH until almost all solids are dissolved. The methylenechloride layer is separated, washed with water, dried with Na2SO4 and concentrated in vacuo to 75 g. of 3-(1,2-difluoro-1,2,2-trichloroethyl)-aniline as yellow oil.

Provenance & Evidence