Sulfuric Acid → N-Nitrosodiphenylamine

Participants

Reaction Steps

210 g of 20% diphenylamine solution in trichloroethylene, 59 g of 38% sodium nitrite aqueous solution and 150 g of 20% sulfuric acid are simultaneously fed, under stirring, (Re = 8-10×103) at 17°-20° C. for about 7-10 min into a 500 ml reactor equipped with a cooling jacket, a thermometer and an agitator; this is followed by another stirring for about 5-8 min. The stirring is discontinued after said period of time has elapsed; complete layer separation of the organic and aqueous phases takes place during 15-20 min. 217 g of organic phase containing 48.4 g of N-nitrosodiphenylamine and 0.42 g of diphenylamine are obtained. Diphenylamine conversion degree is 99%; N-nitrosodiphenylamine yield, 99.3% in terms of converted diphenylamine.

Provenance & Evidence