Organic phosphorus light emitting material and preparation method thereof, and organic electroluminescence device made from organic phosphorus light emitting material
A technology of light-emitting materials and organic phosphorous, applied in the field of organic electroluminescent devices, can solve the problems of high requirements on synthesis process, short life, easy to pollute the environment, etc.
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Embodiment 1
[0060] Embodiment 1 prepares compound L001
[0061]
[0062] ①Under nitrogen protection system, weigh A-001 (2-phenylpyridine 64.5mmol, 10g), IrCl 3 ·3H 2 O (24.8mmol, 8.75g) was put into the reaction system, a mixed solution of 300mL ethylene glycol ether and 100mL pure water was added, refluxed for 24 hours under the protection of nitrogen, and then cooled to room temperature, a precipitate was precipitated, the precipitate was suction filtered, and water , absolute ethanol, and petroleum ether were washed and dried in sequence. The bridging ligand B-001 (6.64 g, yield 50%) was obtained as a yellow powder.
[0063] ②Weigh intermediate B-001 (4.67mmol, 5g), add silver trifluoromethanesulfonate (14mmol, 3.6g), then add 100mL of dichloromethane to the system, add 40mL of methanol, under the protection of nitrogen, reflux for 24 hours , cooled to room temperature, column chromatography (short column) filtrate was concentrated until solid precipitation. The iridium complex...
Embodiment 2
[0068] Embodiment 2 prepares compound L044
[0069]
[0070] ①Under nitrogen protection system, weigh A-044 (52.84mmol, 10g), IrCl 3 ·3H 2 O (21.12mmol, 7.45g) was put into the reaction system, a mixed solution of 300mL ethylene glycol ether and 100mL pure water was added, refluxed for 24 hours under the protection of nitrogen, and then cooled to room temperature, a precipitate was precipitated, the precipitate was suction filtered, and water , absolute ethanol, and petroleum ether were washed and dried in sequence. The bridging ligand B-044 was obtained as a yellow powder (6.8 g, yield 53%).
[0071] ②Weigh intermediate B-044 (4.96mmol, 6g), add silver trifluoromethanesulfonate (14.8mmol, 3.8g), then add 120mL of dichloromethane to the system, add 40mL of methanol, under the protection of nitrogen, reflux for 24 Hours, cooled to room temperature, column chromatography (short column) filtrate concentrated to solid precipitation. The iridium complex intermediate C-044 (7...
Embodiment 3
[0076] Embodiment 3 prepares compound L073
[0077]
[0078] ①Under the nitrogen protection system, weigh raw material A-073 (59.45mmol, 20g), IrCl 3 ·3H 2 O (19.8mmol, 7g) was put into the reaction system, a mixed solution of 500mL ethylene glycol ether and 167mL pure water was added, refluxed for 18 hours under the protection of nitrogen, and then cooled to room temperature. Wash and dry with water ethanol and petroleum ether in sequence. The bridging ligand B-073 (8.5 g, yield 60%) was obtained as a yellow powder.
[0079] ②Then weigh intermediate B-073 (5.9mmol, 8.5g), add silver trifluoromethanesulfonate (17.7mmol, 4.55g), then add 200mL of dichloromethane to the system, add 50mL of methanol, under the protection of nitrogen, reflux After 24 hours, it was cooled to room temperature, and the filtrate was concentrated by column chromatography (short column) until solids were precipitated. The intermediate C-073 (10.1 g, yield 80%) was obtained as a yellow-green powder...
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