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Bis(4-diphenylamino)-<strong>[84-67-3]2,2'-dimethyl-4,4'-diaminobiphenyl</strong> (hereinafter abbreviated as BDDMD) represented by the formula (34) was prepared from p-hydroxydiphenylamine and 4,4'-diaminodiphenyl ether according to the following procedure (white solid, yield of 88percent). [Show Image] In 1 liter of toluene, 10.6145 g (0.05 mols) of <strong>[84-67-3]2,2'-dimethylbenzidine</strong> was dissolved. To obtain a dehydrating condensation agent, 153.144 g (0.45 mols) of titanium tetra-n-butoxide and 67.5765 g (0.45 mols) of p-tolyl acetate were evaporated on a water bath of 60°C for 60 minutes to completely distill off the resulting butyl acetate. This agent was added to the solution. While keeping the reaction solution at 110°C, 22.2264 g (0.12 mols) of p-hydroxydiphenylamine was added to the solution under nitrogen atmosphere, followed by reaction at the temperature for 48 hours under nitrogen atmosphere. After completion of the reaction, the reaction solution, cooled down to room temperature, was filtered and the resulting filtrate was washed with toluene and then with diethyl ether and dried to obtain white powder. The thus obtained crude product of BDDMD was purified according to the treatment with active carbon and recrystallization treatment as in Comparative Example 1. The recovery rate was at 98percent
With bis(tri-t-butylphosphine)palladium(0); sodium t-butanolate; In toluene; at 100℃; for 17h;
To a one-necked flask were added A-1-1 (2.5 g), B8 (3.6 g)And sodium tert-butoxide (4.4 g) was added thereto.Fill the flask, add di-gassed toluene (40 mL), and heat to 100 oC. Pd [P (t-Bu) 3] 2 (200 mg), PdAnd the mixture was stirred at the same temperature for 17 hours.Diluted with DCM (100 mL) and filtered through SiO2.The filtered solution was depressurized to remove the solvent. The solvent was dissolved again in THF to obtain EA, which was then recrystallized to obtain A-8-1 (1.8 g).
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