Nitrobenzene → HCID 19064203, compound

Participants

Reaction Steps

300-ml reactor was charged with 10 q (0.0298 mol) of N,N'-diphenylbenzidie, 25 g (0.0893 mol) of m-iodobiphenyl, 12.3 g (0.0891 mol) of potassium carbonate, 2.6 g of copper powder, and 150 ml of nitrobenzene. In an argon stream, the contents were heated under reflux for 24 hours. At the end of reaction, the insoluble was removed by filtration and the solvent was distilled off from the filtrate. The still residue was purified through a silica gel column with a 5/1 mixture of n-hexane and ethyl acetate, obtaining 15 g of N,N'-diphenyl-N,N'-di(3-biphenylyl)benzidine of primary purity grade (yield 78.89%. It was further purified by recrystallization from toluene and train sublimation, obtaining 10.6 g of a 99.9% pure product (yield 55.6%). Further purification by sublimation yielded a 99,99% pure product.

Provenance & Evidence