Spiro-iridium organic electrophosphorescent material and preparation method thereof
A phosphorescent material, electromechanical technology, applied in luminescent materials, organic chemistry, chemical instruments and methods, etc., can solve the problems of fluorescence quenching, damage device stability, reduce luminous efficiency, etc., and achieve good photoelectric performance and good thermal stability. , the effect of simple synthesis steps
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Embodiment 1
[0034] Embodiment 1: 2-9, the synthesis of 9'-(2-oxanthracenyl) spirofluorene-1,3,2-dioxoboronic acid
[0035] Take 2-bromo-9,9'-(2-oxanthranyl)fluorene (14.64mmol, 6.0211g) into a 500ml two-necked flask, vacuumize and fill with nitrogen, and place the reaction device in a -78 At a low temperature of ℃, take anhydrous and oxygen-free freshly steamed THF to dissolve, add n-butyl lithium (17.57mmol, 10.97mL) dropwise into a two-necked flask, and react at -78℃ for 1h, and then react at room temperature for 1 hour, Quickly add n-butyl borate (73.2mmol, 19.79mL) into the reactor at -78°C, keep the temperature at low temperature for 1h, slowly return to the temperature, and react overnight; three times the amount of dilute hydrochloric acid is hydrolyzed for 3-5h, quenched in an ice-water bath reaction, washed with NaCl, extracted with dichloromethane, dried, and distilled under reduced pressure to obtain a crude product. Transfer it to a 500mL single-necked flask, add 1,3-propaned...
Embodiment 2
[0036] Example 2: Synthesis of 2-pyridyl-9,9'-(2-oxanthracenyl)fluorene
Embodiment 3
[0037] Take 2-9,9'-(2-oxanthranyl)spirofluorene-1,3,2-dioxoborinate (0.5mmol, 0.208g), 2-bromopyridine (0.5mmol, 0.05mL), TBAB Add a little to a 100ml two-necked round bottom flask, vacuumize, add tetraphenylphosphorous palladium, vacuumize, and protect with nitrogen. Add 1mL of 2mol / L potassium carbonate solution, add 5mL of a mixed solution of tetrahydrofuran and toluene, and heat at 90°C for 48h under dark conditions. After the reaction, it was extracted with chloroform, dried over anhydrous magnesium sulfate, concentrated to obtain a crude product, and 0.1820 g of the product was obtained by column chromatography with a yield of 89%. Example 3: Synthesis of 2-pyridyl-9,9'-(2-oxanthracenyl)fluorene and iridium trichloride hydrate dimer 2-pyridyl-9,9'-(2-oxo Xanthenyl) fluorene (1mmol, 0.4090g), iridium trichloride hydrate (0.5mmol, 0.17632g) was added in the reaction flask, vacuumed nitrogen, injected 2-ethoxyethanol and water (volume ratio is 3: 1) and reflux at 120° C. ...
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