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N-Biphenyl-4-yl-N',N'-diphenyl-benzene-1,4-diamine synthesis

1synthesis methods
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Yield:880800-19-1 81.5%

Reaction Conditions:

with tris-(dibenzylideneacetone)dipalladium(0);tri-tert-butyl phosphine;sodium t-butanolate in toluene at 120; for 10 h;Inert atmosphere;

Steps:

6.1 Step 1: Synthesis of Intermediate 53-1

Combine 4-aminobiphenyl (8.2g, 48.5mmol), 4-bromotriphenylamine (15.7g, 48.5mmol),Sodium tert-butoxide (9.3g, 97mmol) was added to the reaction flask and replaced with nitrogen 3 times.Add toluene (100ml) under nitrogen protection, replace with nitrogen 3 times, add tris(dibenzylideneacetone) bispalladium (0.44g, 0.485mmol), 50% tri-tert-butylphosphine (0.39g, 0.97mmol) under nitrogen protection , Nitrogen replacement 3 times, heating to 120°C and stirring for 10h. Cool to room temperature,Add 100ml of water and stir for 30min, suction and filter the solid to dry,The solid compound was separated and purified by column chromatography to obtain 16.3 g, 81.5%.

References:

CN112961134,2021,A Location in patent:Paragraph 0095-0098