Organic light-emitting material with room-temperature phosphorescence performance and preparation method and application thereof
A luminescent material, room temperature phosphorescence technology, applied in luminescent materials, organic chemistry, chemical instruments and methods, etc., can solve the problems of low room temperature phosphorescence quantum yield, limited material types, and no room temperature phosphorescence performance of phosphorescent materials.
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Embodiment 1
[0050] (1) Synthesis of intermediate 4,4'-diiodo-diphenylsulfone, the synthetic route is as follows:
[0051]
[0052] Add iodobenzene (7.0g, 34.3mmol) and chlorosulfonic acid (12.3g, 105.6mmol) into a 250ml round-bottomed flask and react at 50°C for 3 hours. After the reaction, pour the mixture into an ice-water bath and stir thoroughly, and filter Finally, the water layer was removed, the organic layer was washed with water, dried over anhydrous sodium sulfate, and separated by silica gel column chromatography, dichloromethane:petroleum ether=1:1 was used as eluent to obtain 5.96g of yellow-white solid, yield: 74%, The structure is identified as: 4,4'-diiodo-diphenyl sulfone, the theoretical value of elemental analysis is C 12 h 8 I 2 o 2 S (%): C 30.66, H 1.72, O 6.81; found values: C 30.56, H 1.78, O 6.78.
[0053] (2) Synthesis of intermediate 4-iodo-4'-carbazolyl diphenyl sulfone, the synthetic route is as follows:
[0054]
[0055] Select 4,4'-diiodo-diphenyl...
Embodiment 2
[0061] The synthesis of embodiment 2 target product, synthetic route is as follows:
[0062]
[0063] Add 4-iodo-4'-carbazolyldiphenylsulfone (2.00g, 3.93mmol), cuprous cyanide (0.42g, 4.72mmol), 15ml of N,N-dimethylformamide, and add 100ml of round bottom The flask was refluxed overnight, cooled to room temperature, poured into 2ml of ferric chloride hydrochloric acid solution, stirred for half an hour, quenched with 10ml of saturated aqueous sodium chloride solution, extracted with dichloromethane, dried over anhydrous sodium sulfate, and separated by silica gel column chromatography. Dichloromethane is used as eluting agent, the product is white powder, productive rate: 87%, elemental analysis theoretical value C 25 h 16 N 2 o 2 S (%): C 73.51, H 3.95, N 6.86, found values: C 73.38, H 4.05, N 6.92.
[0064] Such as figure 1 As shown, the fluorescence emission peak of the target product in Example 2 in n-hexane is 368nm, and the low-temperature phosphorescence peak i...
Embodiment 3
[0066] (1) Synthesis of intermediate 4-iodo-4'-phenothiazinyl diphenyl sulfone, the synthetic route is as follows:
[0067]
[0068] 4,4'-diiodo-diphenylsulfone (1.50g, 3.19mmol), phenothiazine (0.70g, 3.50mmol), sodium tert-butoxide (0.55g, 5.71mmol), palladium acetate (0.025g, 0.11mmol), tri-tert-butylphosphine tetrafluoroborate (0.095g, 0.33mmol), 50ml of toluene, put into a 100ml round bottom flask, reflux at 110°C for 48 hours, quenched with 10ml of saturated aqueous sodium chloride solution, dichloromethane Extracted, dried over anhydrous sodium sulfate, separated by silica gel column chromatography, dichloromethane / petroleum ether (v:v) = 3:2 as eluent, yield: 72%, elemental analysis theoretical value C 24 h 16 IN 5 o 2 S 2 (%): C 53.24, H 2.98, N 2.59, found values: C 53.36, H 2.78, N 2.47.
[0069] At the same time, the intermediate 4-iodo-4'-phenothiazinyldiphenylsulfone is also one of the target products.
[0070] (2) Synthesis of the target product of embo...
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