Organic light-emitting compound as well as preparation method and application thereof
A technology of light-emitting compounds and compounds, applied in the fields of silicon-organic compounds, organic chemistry, chemical instruments and methods, etc., can solve problems such as different performances
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Embodiment 1
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[0082]Under nitrogen protection, starting material A-1-1 (16.0 g, 50 mmol) and starting material B-1 (9.8 g, 50 mmol) were dissolved in 300 mL of dry toluene in a 500 mL round bottom flask. Then sodium tert-butoxide (9.6g, 100mmol) and 2-dicyclohexylphosphine-2,4,6-triisopropylbiphenyl (4.76g, 10mmol) were added to the flask, followed by palladium acetate (0.56g, 2.5 mmol). The reaction was heated to 100°C and stirred for 10 hours. After the reaction, the temperature was lowered to room temperature, the salt and catalyst were removed, the toluene was concentrated, and 200 mL of ethanol was used for recrystallization to obtain intermediate C-1-1 (16.17 g, yield 80%).
[0083] Table 1 Example 1 reaction raw materials and product structure and characterization summary
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Embodiment 2
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[0088] In a 500mL round-bottomed flask, Intermediate C-1-1 (16.17g, 40mmol) and Intermediate D-1-1 (14.0g, 40mmol) were completely dissolved in a mixed solution of 150mL toluene and 50mL tetrahydrofuran, and then added p-toluenesulfonic acid (8.6 g, 50 mmol), and the resultant was heated to 50° C. and stirred for 2 hours. After the temperature was lowered to room temperature, 100 mL of distilled water and sodium carbonate were added to the reaction solution to neutralize the solution to neutrality. Liquid separation, extraction, and concentration of the organic phase to a little solvent, was added dropwise to cold ethanol, and the precipitated intermediate E-1-1 (19.98 g, yield 90%) was obtained.
[0089] Table 2
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Embodiment 3
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[0094] After the intermediates E-1-1 (19.43g, 35mmol) and F-1-1 (8.12g, 35mmol) were completely dissolved in 300mL of dry toluene in a 500mL round bottom flask under nitrogen protection, tert-butyl Sodium alkoxide (10.07g, 105mmol), then tri-tert-butylphosphine (1.54g, 7mmol) and tris(dibenzylideneacetone)dipalladium (0.32g, 0.35mmol) were added, and the resultant was heated to 100°C and stirred 12 hours. After lowering the temperature to room temperature, the resultant was filtered to remove salt, concentrated toluene, and recrystallized using ethanol to obtain intermediate G-1-1 (18.81 g, yield 76%).
[0095] table 3
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PUM
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