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2-chloro-4-(9-phenyl-9H-carbazol-2-yl)benzo[4,5]thieno[3,2-d]pyrimidine[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
78%
With tetrakis(triphenylphosphine) palladium(0); sodium hydroxide; In 1,4-dioxane; water; at 80℃;
In a round bottom flask, intermediate 1-3 (10 g, 39.2 mmol), (9-phenyl-9H-indazol-2-yl)boronic acid (11.3 g,39.2 mmol), tetrakistriphenylphosphonium (1.4 g, 1.2 mmol), sodium hydroxide (3.9 g, 98 mmol) and tetrahydrofuran (200 mL)Mixed solvent with deionized water (100 mL). The reaction system was heated to reflux at 80 C. After the reaction is completed, it is cooled to room temperature.The reaction solution was diluted with distilled water. The reaction mixture was then extracted with dichloromethane and water.Purification by silica gel chromatography, recrystallization to give intermediate 1-6 (13.6 g, 78%)