Fluorine-containing blue organic luminescent material and preparation method thereof
A luminescent material, organic technology, applied in the direction of luminescent material, organic chemistry, halogenated hydrocarbon preparation, etc., to achieve the effect of easy storage, good color purity and stable structure
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Embodiment 1
[0027] Embodiment 1: The following steps are adopted for the preparation of 9-bromo-3-fluoro-9H-fluorene: 1. In a 50 ml three-necked round-bottomed flask equipped with a magnetic stirrer, a constant pressure dropping funnel, a condensation device and an exhaust gas absorption device, add Add 30 ml of dichloromethane to dissolve 0.21 g of 3-fluoro-9-fluorenol. ② Add 0.12 ml of phosphorus tribromide drop by drop in an ice-water bath. ③After the dropwise addition, react at 0°C for 2 h. ④ Pour the reaction solution into a 100 ml large beaker, slowly add saturated sodium bicarbonate solution under an ice bath, and stir while adding until no more bubbles are generated. The organic phase was washed several times with saturated brine, and dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the obtained crude product was recrystallized from petroleum ether to obtain 0.28 g of light yellow crystals, with a yield of 95.1%.
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Embodiment 2
[0029] Embodiment 2: The following steps are adopted for the preparation of 9-bromo-3-fluoro-9H-fluorene: 1. In a 250 ml three-necked round-bottomed flask equipped with a magnetic stirrer, a constant pressure dropping funnel, a condensation device and an exhaust gas absorption device, add Add 2.48 g of 3-fluoro-9-fluorenol to 150 ml of dichloromethane to dissolve. ② Add 1.2ml of phosphorus tribromide drop by drop in an ice-water bath. ③After the dropwise addition, react at 0°C for 2 hours. ④ Pour the reaction solution into a 500 ml large beaker, slowly add saturated sodium bicarbonate solution under an ice bath, and stir while adding until no more bubbles are generated. The organic phase was washed several times with saturated brine, and dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the obtained crude product was recrystallized from petroleum ether to obtain 3.08 g of light yellow crystals, with a yield of 94...
Embodiment 3
[0031] Example 3: The following steps are used to prepare 9-bromo-3-fluoro-9H-fluorene: 1. In a 1000 ml three-necked round-bottomed flask equipped with a magnetic stirrer, a constant pressure dropping funnel, a condensation device and an exhaust gas absorption device, add 36.3 g of 3-fluoro-9-fluorenol was dissolved in 750 ml of dichloromethane. ② Add 20.8 ml of phosphorus tribromide drop by drop in an ice-water bath. ③After the dropwise addition, react at 0°C for 2 hours. ④ Pour the reaction solution into a 2000 ml large beaker, slowly add saturated sodium bicarbonate solution under an ice bath, and stir while adding until no more bubbles are generated. The organic phase was washed several times with saturated brine, and dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the resulting crude product was recrystallized from petroleum ether to obtain 44.8 g of light yellow crystals, with a yield of 93.8%.
[0032] ...
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