An organic electroluminescent material with oxygen fluorene structure, its preparation method and its application
An electroluminescence, electromechanical technology, applied in the fields of luminescent materials, organic chemistry, chemical instruments and methods, etc., can solve the problems of immature blue light-emitting devices, low device life and efficiency, and achieve high thermal stability and optoelectronic performance. Agglomeration, good film-forming effect
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Embodiment 1
[0043] The preparation of embodiment 1 intermediate 1
[0044] Preparation of Intermediate 1-1: In a 500mL three-necked flask, add methyl 5-bromo-2-iodoformate (34.1g, 0.10mol), dibenzofuran-4-boronic acid (23.3g, 0.11mmol), carbonic acid Potassium (27.6g, 0.20mol), 82.8g water, Pd(PPh 3 ) 4 (578mg, 0.5mmol), toluene (150mL), absolute ethanol (50mL), N 2Protection, heating to reflux, heat preservation reaction, 4 hours, stopping the reaction, cooling to 25°C, separating liquids, collecting the organic phase, washing with water until neutral, and removing the solvent from the organic phase under reduced pressure to obtain the crude product of intermediate 1-1, which is not Refined, directly into the next reaction.
[0045] Preparation of Intermediate 1-2: In a 500mL three-neck flask, add Intermediate 1-1 (38.1g, 0.10mol), sodium hydroxide (12.0g, 0.30mol), absolute ethanol (200mL), N 2 Protect, heat up to reflux, keep warm for 3 hours, cool down to 25°C, add 10% dilute hydr...
Embodiment 2
[0050] The preparation of embodiment 2 compound C02
[0051]
[0052] In a 250mL three-necked flask, add intermediate 1 (6.14g, 10mmol), 1-naphthaleneboronic acid (3.78g, 22mmol), potassium carbonate (4.15g, 30mmol), Pd(PPh 3 ) 4 (58mg, 0.05mmol), mixed xylenes (80mL), N 2 Protect, raise the temperature to reflux, keep the reaction for 8 hours, stop the reaction, lower the temperature to 25°C, add 50mL deionized water, stir for 5min, separate the liquid, collect the organic phase, remove the solvent, and obtain the crude product of CO2, which is purified by silica gel column chromatography , to obtain the target compound C01, with an HPLC purity of 99.83% and a yield of 82.65%. High resolution mass spectrometry, ESI source, positive ion mode, molecular formula C 55 h 32 O, theoretical value 708.2453, test value 708.2456. Elemental analysis (C 55 h 32 O), theoretical value C: 93.19, H: 4.55, O: 2.26, measured value C: 93.17, H: 4.56, O: 2.27.
Embodiment 3
[0053] The preparation of embodiment 3 compound C04
[0054] Carry out with reference to Example 2, the raw materials are intermediate 1 and 4-biphenylboronic acid, to obtain the C04 compound, the HPLC purity is 99.95%, and the yield is 78.52%. High resolution mass spectrometry, ESI source, positive ion mode, molecular formula C 59 h 36 O, theoretical value 760.2766, test value 760.2761. Elemental analysis (C 59 h 36 O), theoretical value C: 93.13, H: 4.77, O: 2.10, measured value C: 93.11, H: 4.76, O: 2.13.
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