HCID 14401596, compound → 1095-78-9

Participants

Reaction Steps

96.7 g (0.23 mol) of 2,2-bis-(3-amino-4-nitrophenyl) hexafluoropropane are dissolved in 1,000 ml of ethyl acetate and reduced with hydrogen (100 bar) at 25° C. in an autoclave after the addition of 3 g of a palladium/charcoal catalyst (5% Pd). After filtering off the catalyst, the ethyl acetate is separated off on the rotary evaporator. The residue is taken up using 1 1 of water and adjusted to a pH of 1 using 1:1 hydrochloric acid. The mixture is then heated to 70°-80° C., 20 g of activated charcoal are added, the mixture is stirred at 70°-80° C. for 15 minutes and the activated charcoal is filtered off. The colorless filtrate is saturated with nitrogen and is adjusted at 10°-20° C. to a pH of 7 using 1:1 ammonia solution under inert gas. The precipitate is separated off, washed well with water and dried to constant weight under reduced pressure. Yield 74 g (0.20 mol); gas chromatographic purity above 99.9%; white solid; m.p. 218°-220° C.

Provenance & Evidence