Diphenyl sulfone-based bipolar blue phosphor host material and preparation method and apparatus thereof
A host material, blue phosphorescence technology, applied in electroluminescent diodes, the field of bipolar blue phosphorescence host materials, can solve the problems such as the structure of blue light devices needs to be simplified, and achieve easy large-scale preparation and high-efficiency device performance , The preparation method is simple and feasible
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Embodiment 1
[0040] Embodiment 1: the preparation of formula 2 compound
[0041] In a 500ml three-necked flask, add 8.91g (30mmol) of 4-bromodiphenylsulfone, 8.4g (33mmol) of pinacol ester of diboronic acid, 8.8g (90mmol) of anhydrous potassium acetate, [1,1'-bis(di Phenylphosphorus)ferrocene]palladium dichloride 1.2g, dioxane 200ml, reflux reaction under nitrogen protection for 24h. Cool to room temperature, add 200ml of water, then extract with dichloromethane (2*200ml), combine the organic layers, dry over anhydrous sodium sulfate, and concentrate to obtain an oil. After column chromatography, the volume ratio of ethyl acetate:petroleum ether=1:20~1:5 was eluted to obtain 8.5 g of white solid with a yield of 82.31%. 1 HNMR (300MHz, CDCl 3 )δ (ppm): 7.94-7.92 (m, 6H), 7.57-7.45 (m, 3H), 1.32 (s, 12H). 1 See attached for HNMR spectrum figure 1 .
Embodiment 2
[0042] Embodiment 2: the preparation of formula 4 compound
[0043] In a 500ml three-necked flask, add 6.05g (17.6mmol) of the compound of formula 2 obtained above, 3.28g (8mmol) of 3,6-dibromo-9-phenylcarbazole, 1.0g of tetrakis(triphenylphosphine)palladium, 20ml of potassium carbonate aqueous solution (4.3g of potassium carbonate dissolved in 20ml of water), 40ml of ethanol and 200ml of toluene were mixed evenly, and the reaction was refluxed under nitrogen protection for 24h. The reaction solution was cooled to room temperature, then extracted with dichloromethane (2*200ml), the organic layers were combined, dried over anhydrous sodium sulfate, and concentrated to obtain an oil. After column chromatography, the volume ratio of ethyl acetate:petroleum ether=1:10~1:3 was eluted to obtain 2.5 g of white solid with a yield of 45.21%. 1 HNMR (300MHz, CDCl 3 )δ (ppm): 8.38 (s, 2H), 8.06-8.00 (m, 8H), 7.85-7.82 (d, J=8.4Hz, 4H), 7.67-7.46 (m, 15H). 1 See attached for HNMR spect...
Embodiment 3
[0044] Embodiment 3: the preparation of formula 6 compound
[0045] In a 500ml three-necked flask, add 6.05g (17.6mmol) of the compound of formula 2 obtained above, 3.28g (8mmol) of 2,7-dibromo-9-phenylcarbazole, 1.0g of tetrakis(triphenylphosphine)palladium, 20ml of potassium carbonate aqueous solution (4.3g of potassium carbonate dissolved in 20ml of water), 40ml of ethanol and 200ml of toluene were mixed evenly, and the reaction was refluxed under nitrogen protection for 24h. The reaction solution was cooled to room temperature, then extracted with dichloromethane (2*200ml), the organic layers were combined, dried over anhydrous sodium sulfate, and concentrated to obtain an oil. After column chromatography, the volume ratio of ethyl acetate:petroleum ether=1:10~1:3 was eluted to obtain 2.7g of white solid with a yield of 48.82%. 1 HNMR (300MHz, CDCl 3 )δ(ppm):8.25-8.22(d,J=8.7Hz,2H),8.04-7.99(t,J=8.1Hz,4.5Hz,8H),7.75-7.78(d,J=8.4Hz,4H) ,7.69-7.53(m,15H). 1 See attached ...
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