Yellow light emitting iridium phosphorescence coordination compound and method for preparing same
A technology of phosphorescent complexes and ligands, which is applied in the direction of luminescent materials, indium organic compounds, platinum group organic compounds, etc., and can solve the problems of low luminous efficiency and short service life
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Embodiment 1
[0021] Synthesis of 2,4-bis(3,5-dimethylphenyl)pyridine:
[0022] Add 2,4-dichloropyridine (18.4g, 124.3mmol), 3,5-dimethylphenylboronic acid (37.0g, 136.73mmol), and tetrakis(triphenylphosphorus) palladium into a 1L three-neck round bottom flask (2.5g, 2.16mmol) and anhydrous sodium carbonate (61.8g, 583.02mmol), then add 200mL tetrahydrofuran and 200mL secondary deionized water, in N 2 Under protection, the reaction was refluxed at 70°C for 24 hours. After cooling to room temperature, the solvent was removed, a large amount of deionized water was added, and dichloromethane extraction was performed three times. Methanol was added to the extracted organic phase, and the precipitated tetrakis(triphenylphosphonium) palladium solid was recovered and the filtrate Use anhydrous MgSO 4 dry. After the solvent was removed by filtration, the residue was passed through the column to obtain 43.2 g of a pale yellow oily substance with a yield of 78%.
[0023] 1. Elemental analysis: Theoretica...
Embodiment 2
[0028] Synthesis of bis-{[2,4-bis(3,5-dimethylphenyl)pyridine]} iridium dichloride:
[0029] Add hydrated iridium trichloride (15.0g, 42.0mmol), 2,4-bis(3,5-dimethylphenyl)pyridine (30.0g, 14.5mmol) into a 500ml three-necked round bottom flask, and then add 270ml Ethylene glycol monoethyl ether and 90ml of secondary deionized water were refluxed at 120°C for 24hrs under the protection of argon. Cooled to room temperature, filtered, the filter cake was washed with ethanol and water, and dried under vacuum at 60°C for 24hrs to obtain bis-{[2,4-bis(3,5-dimethylphenyl)pyridine]} iridium dichloride 28.88g, the yield was 85.6%.
Embodiment 3
[0031] Synthesis of bis[2,4-bis(3,5-dimethylphenyl)pyridine] acetylacetonate iridium:
[0032] Add bis-{[2,4-bis(3,5-dimethylphenyl)pyridine]} iridium dichloride (15.0g, 9.4mmol) and anhydrous sodium carbonate to a 500ml three-necked round bottom flask. 4.95g, 46.9mmol), acetylacetone (2.25g, 20.6mmol), 300mL ethylene glycol monoethyl ether was added, argon was repeatedly pumped three times, and the reaction was refluxed at 135°C for 24h under the protection of argon. After cooling to room temperature, the mixture was poured into a large amount of water, filtered, the filter cake was dried and dissolved in dichloromethane, passed through the column, after removing the solvent, the residue was recrystallized with dichloromethane and methanol to obtain the target product 13.1g, the yield was 87.5 %.
[0033] 1. Elemental analysis: theoretical value (%): C 65.33H 5.48N 3.24,
[0034] Measured value (%): C65.35H 5.47N 3.21
[0035] 2. NMR spectrum: 1 H-NMR(CDCl 3 ,ppm): 8.42 (d, 2H), 8....
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