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With potassium carbonate;tetrakis(triphenylphosphine) palladium(0); In tetrahydrofuran; water; for 6h;Heating / reflux;
Synthesis of Compound 1; 1.85 g of Intermediate 1c (3.90 mmol) and 1 g of Intermediate 1d (3.90 mmol) were added to a mixed solvent of 2.7 g of an aqueous potassium carbonate solution (19.5 mmol) and THF. 225 mg of Pd(PPh3)4 (19.5 mmol) was added to the mixture while the mixture was stirred, and the mixture was refluxed for 6 hours. The mixture was cooled to room temperature, and then the obtained solid compound was filtered while being washed with water, ethanol and THF to obtain 1.73 g of Compound 1 in the form of a pale yellow powder (yield 71%). (1H NMR (400 MHz, CDCl3) 8.13-8.04 (7H), 8.01 (1H), 7.97-7.92 (4H), 7.86-7.82 (2H), 7.75 (2H), 7.71-7.58 (10H), 7.32 (2H), 7.15 (1H), 6.75 (1H)).
71%
With potassium carbonate;tetrakis(triphenylphosphine) palladium(0); In tetrahydrofuran; water; for 6h;Heating / reflux;
Synthesis of Compound 1; 1.85 g of Intermediate 1c (3.90 mmol) and 1 g of Intermediate 1d (3.90 mmol) were added to a mixed solvent of 2.7 g of an aqueous potassium carbonate solution (19.5 mmol) and THF. 225 mg of Pd(PPh3)4 (19.5 mmol) was added to the mixture while the mixture was stirred, and the mixture was refluxed for 6 hours. The mixture was cooled to room temperature, and then the obtained solid compound was filtered while being washed with water, ethanol and THF to obtain 1.73 g of Compound 1 in the form of a pale yellow powder (yield 71%). (1H NMR (400MHz, CDCl3) 8.13-8.04 (7H), 8.01 (1H), 7.97-7.92 (4H), 7.86-7.82 (2H), 7.75 (2H), 7.71-7.58 (10H), 7.32 (2H), 7.15 (1H),6.75(1H)).
With 18-crown-6 ether; potassium carbonate;copper; In 1,2-dichloro-benzene; at 200℃; for 48h;Inert atmosphere;
Into a reactor, 6.1 g (19 mmoles) of <strong>[56525-79-2]3,6-diphenylcarbazole</strong>, 6.3 g (23 mmoles) of Intermediate Compound (A), 0.2 g of copper powder, 1.7 g of 18-crown-6 and 2.9 g (21 mmoles) of potassium carbonate were placed and 30 ml of o-dichlorobenzene was added as the solvent. The resultant mixture was heated at 200° C. in a silicone oil bath under a nitrogen stream and the reaction was allowed to proceed for 48 hours. After the reaction was completed, the reaction mixture was filtered under suction before being cooled and the obtained filtrate was concentrated using an evaporator. To the obtained oily product, 30 ml of methanol was added. The formed solid substance was separated by filtration under a reduced pressure and a gray solid substance was obtained. The obtained solid substance was recrystallized from benzene and 3.0 g (the yield: 31percent) of white crystals were obtained. It was confirmed by 90 MHz 1H-NMR and FD-MS (the field desorption mass analysis) that the obtained crystals were the target substance (A5). The result of the measurement by FD-MS is shown in the following:FD-MS calcd. for C37H25N3=511; found: m/z=511 (M+, 100)
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