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To a 250 mL three-necked flask, 2-bromocarbazole (6.0 g, 24.38 mmol), sodium hydroxide solution (50%) 4 ml, tetrabutylammonium bromide (0.4 g, 1.24 mmol), and the temperature was stirred for 5 min at room temperature. Bromine hexane (8.045 g, 48 mmol) was added dropwise with a syringe.After 12 h of reaction, the eluent was purified by column chromatography to petroleum ether to afford product 1a as an oil, which, after vacuum drying, weighed 7.57 g (yield about 94%).
2-Bromocarbazole (20.1 g, 81.6 mmol) and triphenylene-2-boronic acid (23 g, 84.5 mmol) were dissolved in tetrahydrofuran (200 ml), potassium carbonate (K2CO3, potassium carbonate, 40.4 g, 292.8 mmol)Was added to the reaction solution together with water, and the mixture was heated and stirred in a nitrogen state for about one hour.After stirring for one hour, tetrakis (triphenylphosphine) palladium (2.3 g, 1.95 mmol) was added and the mixture was heated with stirring for 6 hoursAfter completion of the reaction, the temperature was lowered to room temperature, and tetrahydrofuran was removed by distillation under reduced pressure, followed by filtration under reduced pressure. The solid obtained by filtration was recrystallized from tetrahydrofuran and ethanol to obtain the formula P1 (28 g, yield 87%)
81%
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; for 12h;Inert atmosphere; Reflux;
2-bromo-carbazole (10.0 g, 40.6 mmol),Triphenylene2-boronic acid (13.2 g, 48.5mmol), and potassium carbonate (17.0 g, 123mmol) and tetrahydrofuran (100 mL) and a mixture of water (50 mL) was suspended within. After filling nitrogen,Tetrakis (triphenylphosphine) palladium (0.9 g, 0.7 mmol) was added to the suspension. Under nitrogen, the mixture was stirred for about 12 hours at reflux.After cooling to room temperature the resulting solids were filtered. To a pale yellow solid of the purified using a THF / EtOH P1 of white solid (13 g, 81%) was obtained.
4-(9H-carbazol-2-yl)-N,N-diphenylaniline[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
91%
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; at 80℃; for 12h;
General procedure: 3-bromo-9H-carbazole (492.21 mg, 2 mmol), <strong>[267221-88-5]N,N-diphenyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline</strong> (965.35 mg, 2.6mmol), potassium carbonate (414.63 g, 3 mmol), terakis(triphenylphosphine)palladium (115.56 mg, 0.1 mmol) were dissolved in amixture solution of tetrahydrofuran (15 ml) and water (5 ml) andrefluxed under nitrogen at 80 C for 12 h. Then, the mixture wasextracted with dichloromethane and washed with water. The organiclayer was dried over anhydrous MgSO4 and the residue was purified on asilica gel column using petroleum ether/dichloromethane mixture (3:1,v/v) as eluent to afford the product as white powder (1180.6 mg, yield:89%).
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