An organic electroluminescent compound
An electroluminescence and compound technology, applied in the field of organic electroluminescence compounds, can solve the problems of poor device efficiency and life, unsatisfactory users, short blue light wavelength, etc., and achieve long life, development promotion, high color purity Effect
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Embodiment 1
[0061] Example 1 Preparation of Compound 4
[0062]
[0063] Step 1: Synthesis of Intermediate 1
[0064]
[0065] Dissolve raw material 1 (30.7 g, 120 mmol) and methyl o-bromobenzoate (10.8 g, 50 mmol) in 200 ml of toluene solution, then add 60 ml of 2M aqueous sodium carbonate solution and 60 ml of ethanol, and use After nitrogen exhaust for 30 minutes, add catalyst tetrakis (triphenylphosphine) palladium (Pd(PPh 3 ) 4 (3.5 g, 3 mmol), under stirring conditions, heated to 100 ° C, reacted for 24 hours; when cooled to room temperature, added dichloromethane and deionized water, extracted the organic phase, dried with anhydrous magnesium sulfate, filtered, and reduced pressure , concentration, separation and purification with a silica gel column to obtain about 16.6 g (38.0 mmol) of pure intermediate 1, and the yield is about 76%.
[0066] High-resolution mass spectrometry HRMS [ESI + ] m / z = 436.1324 (theoretical value is 436.1311).
[0067] Step 2: Synthesis of In...
Embodiment 2
[0087] Example 2 Preparation of Compound 25
[0088]
[0089] Steps 1 to 4: Synthesis of Intermediates 1-4
[0090] The synthesis method and specific steps of intermediate 1-4 are the same as those in Example 1.
[0091] Step 5: Synthesis of intermediate 10
[0092]
[0093] 4-tert-butylaniline (7.4 g, 50 mmol), p-cyanobromobenzene (9.0 g, 50 mmol), bis(dibenzylideneacetone) palladium (862 g, 1.5 mmol), tri-tert-butylphosphine (606 mg, 3 mmol) were added together to toluene (100 ml), heated to 90°C under argon flow, followed by adding sodium tert-butoxide (288 mg, 3 mmol), and continued heating to 100°C, stirred and reacted for 12 hours. The reaction solution was cooled to room temperature, and water was added for liquid separation; the obtained organic layer was concentrated, and the obtained solid was purified by silica gel column chromatography to obtain intermediate 10 (10.0 g, 40 mmol), with a yield of 81%.
[0094] Mass spectrum MS of intermediate 10 [ESI + ] ...
Embodiment 3
[0099] Example 3 Preparation of Compound 16
[0100]
[0101] Step 1: Synthesis of Intermediate 5
[0102]
[0103] Dissolve raw material 2 (27.2 g, 100.0 mmol) and methyl o-bromobenzoate (8.6 g, 40.0 mmol) in 250 ml of toluene solution, then add 40 ml of 2M aqueous sodium carbonate solution and 40 ml of ethanol, and After degassing for 30 minutes, add catalyst tetrakis (triphenylphosphine) palladium (Pd(PPh 3 ) 4 (2.8 g, 2.4 mmol), under stirring conditions, heated to 100 ° C, reacted for 36 hours, cooled to room temperature; then, added dichloromethane and deionized water, extracted the organic phase, dried with anhydrous magnesium sulfate, filtered , concentrated under reduced pressure, separated and purified with a silica gel column, and the eluent was petroleum ether / dichloromethane=1:1 (V / V), to obtain about 15.4 g (34.0 mmol) of pure intermediate 5, and the yield was about 85 %.
[0104] Mass spectrum MS of intermediate 5 [ESI + ] m / z = 452.1096 (theoretical va...
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