6.3 g |
With tris-(dibenzylideneacetone)dipalladium(0); tri-tert-butyl phosphine; sodium t-butanolate; In toluene; for 15.0h;Reflux; Inert atmosphere; |
The specific purification method is as follows: 10 g of the crude triarylamine compound of the formula: VI is added to 800 g of a mixture of mass ratios such as mesitylene and meta-xylene. Under the ultrasonic assisted condition of ultrasonic power of 100 W and frequency of 53 kHz, the mixed system was placed at a dissolution temperature of 80 C to completely dissolve the triarylamine compound; 800 g of propionic acid was added to the mixed system, the temperature of the system was maintained at 30 C, ultrasonic assisted crystallization was continued for 0.5 h, filtered, washed with ethanol, and dried to obtain 6.3 g of a white crystal pure product. The yield of the present example was 63%. The purity of the pure triarylamine compound was 99.55% by phase chromatography.The preparation method of the crude triarylamine compound represented by the formula VI in the present embodiment is as follows: Under a nitrogen atmosphere, in a 500 mL three-necked flask, Add 4,4'-dibromobiphenyl (5 g, 16 mmol), N1-(1-naphthyl)-N4,N4-diphenylbenzene-1,4-diamine (12.7 g, 32.8 mmol), Sodium tert-butoxide (6.15 g, 64 mmol), tris(dibenzylideneacetone)dipalladium (0.29 g, 0.32 mmol), 10% tri-tert-butylphosphine in toluene (2.59 g, 1.28 mmol) and toluene 300 mL. After cooling to 60 C, 100 mL of water was added, and the mixture was washed with hot water, dried over anhydrous magnesium sulfate, and evaporated to dryness to dryness to afford 14.3 g of the crude triarylamine compound of formula VI, yield 96.7%, purity 92.3%. |