Tetrahydroanthracene compound containing terpyridyl group and application thereof
An organic and organic material technology, applied in the field of organic electroluminescence display, can solve the problems of increasing the complexity of the device manufacturing process, reducing the cost of OLED, and disadvantages
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[0080] (2) Preparation of Intermediate C:
[0081]
[0082] Under N2 protection, dissolve 20.8g (0.1mol) 9,10-dianthraquinone in 200mL THF dried with Na / benzophenone, cool to -40°C, and slowly add freshly prepared phenyl Grignard reagent THF dropwise The solution (prepared from 39.3g (0.25mol) of bromobenzene and 7.2g of magnesium (0.30mol)) was added dropwise, slowly warmed to room temperature, and continued to stir for 2h. The reaction solution was slowly poured into a saturated ammonium chloride solution, the product was extracted with 200mL ether, the organic phases were combined, and dried with anhydrous MgSO4, and the crude product was subjected to column chromatography to obtain a white solid C-130g (82%) as cis-trans isomerism mixture. Dissolve C-118.2g (0.05mol) in 100mL of benzene, heat to reflux, slowly add 25mL of acetyl chloride through a constant pressure dropping funnel, after the addition is complete, continue to reflux, and detect the reaction by TLC. Aft...
Embodiment 1
[0092] The synthesis of embodiment 1 compound 1
[0093]
[0094] Under the protection of nitrogen, compound B 7.95g (0.01mol), compound D17.65g (0.05mol), Pd (PPh 3 ) 4 Catalyst 0.462g (0.4mmol), potassium carbonate 17.25g (0.125mol) dissolved in 200mL toluene, 150mL ethanol, 100mL water. After pumping and exchanging air three times with a water pump, reflux under nitrogen protection, and monitor the reaction process with a TLC plate. After about 8 hours of reaction, the plate was spotted, and the reaction was complete. After cooling to room temperature, filter with suction, wash the solid with water and hot water, and dry the solid. The solid was dissolved by heating with toluene, hot filtered and a small amount of silica gel was added. The filtrate was concentrated and cooled to room temperature, and filtered to obtain a light yellow solid product. Purification was repeated until the purity was 99.20%, and 10.2 g of light yellow powder was obtained. Product MS (m / e)...
Embodiment 2
[0095] The synthesis of embodiment 2 compound 2
[0096]
[0097] Install a reflux condenser and a nitrogen protection device on a three-necked flask. Under nitrogen protection, add 6.4 grams of compound C (molecular weight 640, 0.01mol), compound D 8.83 grams (molecular weight 353, 0.025mol), Pd (PPh 3 ) 4 Catalyst 0.231 gram (molecular weight 1155, 0.0002mol), potassium carbonate 8.63 gram (molecular weight 138, 0.063 mol), 160ml toluene, 120ml ethanol, 80m water. After pumping and exchanging air for three times with a water pump, reflux under the protection of nitrogen, and monitor the reaction process with a TLC plate. After about 8 hours of reaction, the plate is spotted, and the reaction is complete. After cooling to room temperature, filter with suction, wash the solid with water and ethanol, and dry the solid. The solid was dissolved by heating with toluene, hot filtered and a small amount of silica gel was added. The filtrate was concentrated and cooled to room...
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