Azulene derivative
A derivative, chamomile technology, applied in the field of organic electroluminescent compounds, can solve the problems of large hole transport layer voltage drop, complex industrial production process, low glass transition temperature, etc., to achieve high device efficiency and excellent market potential , the effect of high glass transition temperature
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Embodiment 1
[0051] Example 1 Preparation of Compound 1
[0052]
[0053] Add Intermediate 1 (5.7g, 20.0 mmol) and Intermediate 2 (13.0g, 45mmol), and 10ml of 2M aqueous sodium carbonate and 10ml of tetrahydrofuran into a round-bottomed flask containing 200 ml of toluene, and vent with argon. After 30 minutes, the catalyst tetrakis (triphenylphosphine) palladium (140 mg, 1.2 mmol) was quickly added, and the temperature was raised to 90 ° C under stirring conditions, and the reaction was carried out for 12 hours, and then cooled to room temperature; then ethyl acetate and deionized water were added , extract and combine the organic phases, and dry with anhydrous magnesium sulfate, reduce pressure, concentrate, and finally use silica gel column chromatography, the eluent is petroleum ether: dichloromethane=3:1, to obtain pure compound 1 (10.9 g, 17.8mmol), the yield was 89%.
[0054] High resolution mass spectrum (FAB) of compound 1 (C46H34N2) (m / z): [M] + The detected value is 614.2722...
Embodiment 2
[0055] Example 2 Preparation of Compound 3
[0056] Step 1: Synthesis of Intermediate 6
[0057]
[0058] Intermediate 4 (8.5 g, 50 mmol) and Intermediate 5 (12.4 g, 50 mmol) were dissolved in 200 ml of toluene, and after stirring for 30 minutes, sodium tert-butoxide (480 mg, 5mmol), 3-tert-butylphosphine (1.1g, 5mmol) and bis(dibenzylideneacetone) palladium (864 mg, 1.5 mmol), heated to 100°C, reacted overnight, cooled to room temperature, added water and dichloro Stir with methane, extract and combine the organic phases, dry with anhydrous sodium sulfate, concentrate under reduced pressure, and finally use silica gel column chromatography with petroleum ether as the eluent to obtain pure intermediate 6 (12.5 g, 37.5 mmol). The yield 75%.
[0059] HRMS (FAB) (m / z) of Intermediate 6 (C24H17NO): [M] + The detected value is 335.1310 and the theoretical value is 335.1320.
[0060] Step 2: Synthesis of Intermediate 7
[0061]
[0062] Intermediate 6 (12.5g, 37.5 mmol) ...
Embodiment 3
[0072] Example 3 Preparation of Compound 6
[0073]
[0074] Add intermediate 3 (5.7 g, 20.0 mmol) and intermediate 2 (13.0 g, 45 mmol), and 10 ml of 2M aqueous sodium carbonate solution and 10 ml of tetrahydrofuran into a round-bottomed flask filled with 200 ml of toluene, and argon After degassing for 30 minutes, the catalyst tetrakis(triphenylphosphine)palladium (140 mg, 1.2 mmol) was quickly added, and the temperature was raised to 90 ° C under stirring conditions. After 12 hours of reaction, it was cooled to room temperature, and ethyl acetate and deionized water, extract and combine the organic phases, and dry with anhydrous magnesium sulfate, concentrate under reduced pressure, and finally use silica gel column chromatography, the eluent is petroleum ether: dichloromethane=3:1, to obtain pure compound 6 (11.3g, 18.4mmol), the yield was 92%.
[0075] High resolution mass spectrum (FAB) of compound 6 (C46H34N2) (m / z): [M] + The detected value is 614.2722 and the theo...
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