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With palladium diacetate; caesium carbonate; XPhos; In ethanol; water; toluene; at 110℃; for 3h;Inert atmosphere;
Under a nitrogen stream A13 2.7 g (7.5 mmol), 2.7 g (11.3 mmol) of 2-chloro-4-phenylquinazoline, 0.1 g (5 mol%) of Pd (OAc) 2, xphos, 3.6 g (7.5 mmol) 4.9 g (15.0 mmol) of cesium carbonate and 90 ml / 30 ml / 30 ml of toluene / H2O / ethanol were added and stirred at 110 C for 3 hours. After completion of the reaction, the organic layer was separated using methylene chloride, and water was removed using MgSO4. After removing the solvent of the organic layer, the residue was purified by column chromatography to obtain the target compound R81 (2.3 g, 5.3 mmol, yield 71%).
With potassium carbonate; In N,N-dimethyl-formamide; at 140℃; for 5h;
In the reaction flask, add 7-bromo-benzocarbazole 29.5g (100mmol), 2-chloro-4-phenylquinazoline 16.5g (110mmol), DMF 500mL and potassium carbonate 43.3g (314mmol), at 140 C reaction 5h; the reaction was stopped after the reaction was completed, and the reaction was cooled to room temperature, filtered with water, the resulting solid was purified by toluene recrystallization, to obtain a white powder M1;
Dissolve 9-bromo-7H-benzo[C]carbazole (10.0g, 33.78mmol) in 500ml of DMF, then add sodium hydride (2.7g, 67.56mmol), then add 2-chloro-4-benzene Quinazoline (9.76 g, 40.54 mmol) was stirred at room temperature overnight. After the reaction was completed, distilled water was added to precipitate a solid, which was filtered to obtain the solid, and washed with distilled water and ethanol in turn to obtain a gray solid intermediate A (15 g, yield 89%).
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In 1,4-dioxane; water; for 3h;Reflux;
Combine S2 (30mmol), 2-chloro-4-phenylquinazoline (60mmol), potassium carbonate (45mmol), dioxane (200mL), tetrakis (triphenylphosphine) palladium (0.3mmol), water 50mL Add to the reaction flask, heat to reflux and react for 3 hours. TLC monitors the completion of the reaction. The reaction solution is poured into water and filtered. After extraction with dichloromethane, it is concentrated and recrystallized with toluene to obtain Intermediate A.
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