Soluble functional carbazole derivant, preparation method and application thereof
A carbazole derivative, soluble technology, applied in the field of soluble functional carbazole derivatives, to achieve good thermal stability, high film shape stability, and simple synthesis
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Embodiment 1
[0032] Example 1, 2-(p-(2-ethylhexyloxy)phenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborane
[0033]
[0034] p-(2-Ethylhexyloxy)bromobenzene (5.68g, 20mmol) was dissolved in 80mL of dry tetrahydrofuran, protected, and cooled to -78°C with liquid nitrogen / isopropanol. 2.5M n-BuLi (10 mL, 25 mmol) was slowly added dropwise into the reaction flask, and the mixture changed from colorless to yellow. After the dropwise addition, continue to stir at -78°C for 1h, then add 4,4,5,5-tetramethyl-1,3,2-isopropanol borate (4.65g, 25mmol) with a syringe, yellow Disappeared immediately, then naturally warmed to room temperature and stirred for 24h. The mixture was washed with distilled water and CH 2 Cl 2 Extracted 3 times, the organic phase was extracted with MgSO 4 Let dry overnight. After the solvent was distilled off under reduced pressure, petroleum ether / CH 2 Cl2 Column chromatography gave a colorless oily liquid.
Embodiment 2
[0035] Embodiment 2,3, the preparation of 6-two pairs of (2-ethylhexyloxy) phenylcarbazoles:
[0036]
[0037] 2-(p-(2-ethylhexyloxy)phenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborinane (6.6g, 10mmol), 3, Add 6-dibromocarbazole (1.35g, 4.17mmol), toluene (40mL), ethanol (20mL), and 2M aqueous sodium carbonate solution (20mL) into a two-necked flask, and blow nitrogen gas to exhaust it for 30min. Catalytic amount of Pd(PPh 3 ) 4 (0.1g, 0.09mmol) was quickly added to the reaction flask, and then heated to 80°C for reflux for 12h. After the mixture was cooled, it was washed with distilled water and then washed with CH 2 Cl 2 Extracted 3 times, the organic phase was extracted with MgSO 4 dry. Column chromatography followed by recrystallization gave a white solid.
Embodiment 3
[0038] Embodiment 3,3, the preparation of 6-two p-tert-butylphenylcarbazole:
[0039]
[0040] 2-p-tert-butylphenyl-4,4,5,5-tetramethyl-1,3,2-dioxaborinane (0.65 g, 2.5 mmol), 3,6-dibromocarbazole ( 0.325g, 1mmol), toluene (20mL), ethanol (10mL), and 2M sodium carbonate aqueous solution (10mL) were added into a two-neck flask, and nitrogen gas was bubbled to exhaust for 30min. Catalytic amount of Pd(PPh 3 ) 4 (46mg, 0.03mmol) was quickly added to the reaction flask, and then heated to 80°C for reflux for 12h. After the mixture was cooled, it was washed with distilled water and then washed with CH 2 Cl 2 Extracted 3 times, the organic phase was extracted with MgSO 4 dry. Column chromatography followed by recrystallization gave a white solid.
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