Low temperature method for preparing derivative of tri-arylamine group and application
A derivative, triarylamine technology, applied in the field of electronic materials, can solve the problems of product yield, low purity, high cost, difficult to batch preparation and the like
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example 1
[0022] The synthesis of example one NPD
[0023] Add toluene (340ml), diiodobiphenyl (162.4g, 0.4mol), phenyl-α- Naphthylamine (350.9 g, 1.6 mol), potassium hydroxide flakes (180 g, 3.2 mol), copper powder (25.4 g, 0.4 mol) and 1,10-phenanthroline (7.92 g, 0.04 mol). After the materials are roughly stirred evenly, the reaction device is replaced with nitrogen and kept under an inert atmosphere during the subsequent process;
[0024] Turn on the heat source to heat, and start stirring when the internal temperature reaches 105-110°C, and the contents will soon turn brownish red; when the internal temperature reaches 125-130°C, the contents will reach a stable reflux, and maintain this state for 5 hours. It can be observed that water is continuously condensing in the trap. After the reaction is finished, when the internal temperature is cooled below 100°C, add 200ml of toluene and 200ml of deionized water under stirring, filter the reactant under reduced pressure while it is ho...
example 2
[0025] The synthesis of example two TPD
[0026] Add toluene (65ml), diiodobiphenyl (30.45g, 0.075mol) and m-methyldiphenylamine in sequence to a 250ml three-necked round-bottomed flask equipped with a mechanical stirrer, a thermometer, a condenser tube with a water separator, and a nitrogen port. (30.24 g, 0.165 mol), potassium hydroxide flakes (33.67 g, 0.6 mol), copper powder (4.76 g, 0.075 mol) and 1,10-phenanthroline (1.49 g, 0.0075 mol). After the materials are roughly stirred evenly, replace the reaction device with nitrogen and maintain an inert atmosphere during the subsequent process; turn on the heat source to heat, and start stirring after the internal temperature reaches 105-110°C, and the contents will soon turn purple-black; when The internal temperature reached 125-130°C, and the content reached a steady reflux. The reaction was maintained at this state for 5 hours. During this period, water was continuously condensed in the water separator. After the reaction...
example 3 B
[0027] Synthesis of Example 3 CBP
[0028]Add xylene (60ml), diiodobiphenyl (20.3 grams, 0.05mol), carbazole (25.1 grams, 0.15mol), sheet potassium hydroxide (19.7 grams, 0.35mol), copper powder (3.2g, 0.05mol) and 1,10-phenanthroline (0.99g, 0.005mol). After reaction at 145° C. for 5 hours, 19.5 grams of light earth brown powder were obtained with a yield of 80.0% under similar reaction conditions and post-treatment process as in Example 2. The test shows that it is mainly the product CBP, and the product can be directly sublimated for further refinement.
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