Metal complex, preparation method thereof and application of metal complex in organic electroluminescence devices
A metal complex, electromechanical technology, applied in electric solid devices, chemical instruments and methods, electrical components, etc., can solve problems such as the stability of blue light devices, improve intermolecular stability and luminescence performance, overcome carrier Effects of Unbalanced, Low Bandgap Width
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Embodiment 1
[0068] [Example 1] Synthesis of compound 3-1
[0069] * Preparation of Intermediate 3-1-A
[0070]
[0071] Pyridine-2-boronic acid (2.08g, 16.9mmol), 2,3-diiodobenzene (5.58, 16.9mmol), tetrakistriphenylphosphine palladium (0.7g, 1.08mmol), potassium carbonate (5.3g , 38.3mmol), toluene 500mL, ethanol 40mL and distilled water 40mL, stirred at 70°C for 3h. After the reaction was completed, distilled water was added to stop, and the reactant was extracted with ethyl acetate. The organic layer was dried over MgSO4. The solvent was distilled off under reduced pressure, and purified by silica gel column to obtain compound 3-1-A (2.38g, 50%).
[0072] * Preparation of intermediate 3-1-B
[0073]
[0074] Add pyridine-2-boronic acid (2.08g, 16.9mmol), m-bromoanisole (3.16, 16.9mmol), tetrakistriphenylphosphine palladium (0.7g, 1.08mmol), potassium carbonate (5.3g, 38.3mmol) to the reaction vessel ), toluene 500mL, ethanol 40mL and distilled water 40mL, stirred at 90°C for...
Embodiment 2
[0087] [Example 2] Synthesis of Compound 3-7
[0088] *Synthesis of intermediate 3-7-A
[0089]
[0090] 3-1-A (57.2mmol, 16.08g), aniline (27.24mmol, 2.54g) were added to a 250mL three-necked flask, and tris(dibenzylideneacetone) bispalladium (1.7mmol, 0.98g) was added under nitrogen, tert-butyl Sodium alkoxide (114.2 mmol, 11 g) and toluene 100 mL were stirred at room temperature for 30 min, then tri-tert-butylphosphine (11.4 mmol, 2.3 g) was added under nitrogen protection and the temperature was raised to 80°C for 20 h. Post-treatment: extraction, evaporation of the organic phase to dryness and recrystallization with petroleum ether, the crude product was subjected to column chromatography, the eluent was petroleum ether / dichloromethane = 5:1, the product 3-7-A was evaporated to dryness of the organic phase (6.31 g, 58%).
[0091] *Synthesis of Intermediate 3-7-B
[0092]
[0093] Add 3-7-A (1.71g, 4.29mmol) into a 50mL three-necked bottle, N 2 15 mL of ethylene ...
Embodiment 3
[0097] [Example 3] Synthesis of Compound 3-10
[0098] * Preparation of Intermediate 3-10-A
[0099]
[0100] 3-1-A (23.83g, 84.77mmol) was dissolved in tetrahydrofuran (500mL), cooled to -78°C, n-BuLi (2.5M / 33.9mL, 84.77mmol) was slowly added dropwise, and stirred for 1h. Dimethyldichlorosilane (4.92 g, 38.14 mmol) dissolved in tetrahydrofuran (50 mL) was slowly added dropwise. Stir for another 12 h at room temperature, extract the organic matter with ethyl acetate, and dry the organic layer with MgSO4. The solvent was distilled off under reduced pressure, and purified with a silica gel column to obtain compound 3-10-A (18.64 g, 60%).
[0101] * Preparation of Intermediate 3-10-B
[0102]
[0103] 3-10-A (1.57g, 4.29mmol) into a 50mL three-necked bottle, N 2 15 mL of ethylene glycol ether, 5 mL of water, and 0.6 g (1.71 mmol) of iridium trichloride were added, and the temperature was raised to 100° C. for 17 hours of reaction. Post-treatment, lower the temperature,...
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