N,N'-diphenyl-N,N'-di(9,9-dimethyl fluorene-2-yl)-N-hexyl-(4,4'-diamine phenyl) carbazole and synthetic method thereof
A kind of technology of diaminophenyl and dimethyl fluorene, applied in the field of organic synthesis
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[0026] (1) Synthesis of 2,7-dibromo-N-hexylcarbazole (a)
[0027] Under the protection of argon, 4.88g (15mmol) of 2,7-dibromocarbazole, 0.72g of sodium hydride, and 30mL of DMSO solvent were sequentially added to a 100mL three-necked flask, and the reaction temperature was controlled at 20-30°C, and 1-bromocarbazole was added dropwise. n-Hexane, HPLC detects that the reaction is complete. Quench with 100mL of water, extract with 100mL of dichloromethane, separate layers, extract the aqueous layer with 50mL of dichloromethane, combine the organic phases, dry over anhydrous magnesium sulfate, recover the solvent under reduced pressure to obtain a solid crude product, and carry out extraction with dichloromethane-methanol After recrystallization, 5.87 g of white product 2,7-dibromo-N-hexylcarbazole was obtained, with a purity of 99.8% (HPLC), a yield of 95.6%, and a melting point of 70.6-72.5°C. 1 HNMR (400MHz, CDCl 3 ), δ: 0.858-0.906 (3H, t), 1.295-1.351 (6H, m), 1.786-1.885...
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