A kind of boron material and its preparation method and application
A host material, phosphorescent device technology, applied in chemical instruments and methods, semiconductor/solid-state device manufacturing, electrical components, etc., to achieve the effect of increasing the molecular weight of the compound, good hole/electron balance ability, and reducing the degree of conjugation
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Embodiment 1
[0027] A preparation method of boron material, the steps of the method are as follows:
[0028] Step 1: Dissolve 3.00g of 3-bromospirofluorene ring-closed triphenylamine in anhydrous tetrahydrofuran under the protection of nitrogen, cool to -78°C, and then add 3.9mL of n-butyllithium dropwise. Reaction at ℃ for 1h;
[0029] The second step: add a tetrahydrofuran solution containing 2.49 g of bis(trimethylphenyl)boron fluoride to the reaction system of the first step, react at a temperature of -78°C for 2 hours, then raise the temperature to room temperature, and react at room temperature for 12 hours;
[0030] The third step: add water to the reaction system of the second step to quench the reaction, then wash with water, then extract the organic layer with dichloromethane, then dry the organic layer with anhydrous sodium sulfate, then spin dry, and use a volume ratio of 1 :5 dichloromethane / petroleum ether passes through the column, spins dry again, recrystallizes, obtains t...
Embodiment 2
[0033] A preparation method of boron material, the steps of the method are as follows:
[0034] Step 1: Dissolve 4.00g of 4-bromospirofluorene ring-closed triphenylamine in anhydrous tetrahydrofuran under the protection of nitrogen, cool to -78°C, and then add 5.2mL of n-butyllithium dropwise. Reaction at ℃ for 1h;
[0035] The second step: add a tetrahydrofuran solution containing 3.32 g of bis(trimethylphenyl)boron fluoride to the reaction system of the first step, react at a temperature of -78°C for 2 hours, then raise the temperature to room temperature, and react at room temperature for 12 hours;
[0036] The third step: add water to the reaction system of the second step to quench the reaction, then wash with water, then extract the organic layer with dichloromethane, then dry the organic layer with anhydrous sodium sulfate, then spin dry, and use a volume ratio of 1 :5 dichloromethane / petroleum ether passes through the column, spins dry again, recrystallizes, obtains t...
Embodiment 3
[0039] A preparation method of boron material, the steps of the method are as follows:
[0040] Step 1: Dissolve 4.50g of 3-bromospirofluorene in anhydrous tetrahydrofuran under the protection of nitrogen, cool to -78°C, then add 5.7mL of n-butyllithium dropwise, and react at -78°C 1h;
[0041] The second step: add a tetrahydrofuran solution containing 3.98 g of bis(trimethylphenyl)boron fluoride to the reaction system of the first step, react at a temperature of -78°C for 2 hours, then raise the temperature to room temperature, and react at room temperature for 12 hours;
[0042] The third step: add water to the reaction system of the second step to quench the reaction, then wash with water, then extract the organic layer with dichloromethane, then dry the organic layer with anhydrous sodium sulfate, then spin dry, and use a volume ratio of 1 :5 dichloromethane / petroleum ether passes through the column, spins dry again, recrystallizes, obtains the SF-3-DMB boron material of ...
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