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With sodium carbonate;tetrakis(triphenylphosphine) palladium(0); In water; for 8h;Inert atmosphere; Reflux;
(1) Synthesis of 2-(2-anthryl)triphenylene Under an argon atmosphere, 7.79 g of triphenylene-2-boronic acid piconal ester, 5.14 g of 2-bromoanthracene, 0.462 g of tetrakis(triphenylphosphine)palladium (0), 30 mL of 1,2-dimethoxyethane and 15 mL of a 2M sodium carbonate aqueous solution were placed in a flask, and refluxed with stirring for 8 hours. After cooling to room temperature, deposited crystals were collected by filtration. The resulting solid was subjected to repeated recrystallization with toluene-hexane and washing to obtain 6.07 g (yield: 75%) of 2-(2-anthryl)triphenylene.
After 1-1 (25.71 g, 100.00 mmol) was dissolved in anhydrous THF, the temperature was lowered to -78 C.Add 100 mmol of n-butyllithium and react under nitrogen for 1 hour.Add 1-2 (33.94g, 100.00mmol) and replace it three times with argon.The temperature was gradually raised to room temperature and the reaction was continued for 6 hours. After the reaction is completed, the deionized water is poured and the crude product is precipitated.Filtration, rinsing with water, drying and column chromatography to give 41.28 g of Compound 1,The yield was 85.79%.
With trifluorormethanesulfonic acid; palladium diacetate; silver trifluoroacetate; acetic acid; glycine; at 100℃; for 24h;Sealed tube;
General procedure: A sealed tube with magnetic stir bar was charged with substrate 1 (0.24 mmol), glycine (0.1 mmol, 7.5 mg), Pd(OAc)2 (0.02 mmol, 4.45 mg), AgTFA (0.24 mmol, 53.01 mg) and 2 (0.2 mmol) under air. After addition of AcOH (2 mL) as solvent, TfOH (0.1 mmol, 15.0 mg) was added. The reaction mixture was allowed to stir at 100 C for 24 hours. Upon completion, the reaction mixture was cooled to room temperature, diluted with DCM, and then extracted with saturated NaHCO3 aqueous solution. The organic layer was dried over anhydrous Na2SO4 and concentrated in vacuo. The crude residue was purified by column chromatography on silica gel using PE as the eluent to afford the desired products.
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