反应详情

In a stream of argon, 1.20 g of 2-(3-bromophenyl)-4,6-diphenyl-1,3,5-triazine, 1.30 g of 2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,10-phenanthroline, 1.11 g of cesium carbonate, 14 mg of palladium acetate and 32 mg of triphenylphosphine were suspended in 140 mL of tetrahydrofuran. The suspension was heated under reflux for 19 hours. Then the reaction mixture was left to be cooled to room temperature, and distilled under a reduced pressure to remove low-boiling point ingredients. Methanol was added to the residue, and the deposited solid was collected by filtration. The thus-obtained crude product was purified by silica gel column chromatography using a methanol/chloroform (1:100 to 1:77) mixed solvent as a developing solvent to give 1.37 g of target 4,6-diphenyl-2-[3-(1,10-phenanthrolin-2-yl)phenyl]-1,3,5-triazine as a white solid (yield, 91%).

1. temperatureThe suspension was heated
2. temperatureunder reflux for 19 hours
3. waitThen the reaction mixture was left
4. distillationdistilled under a reduced pressure
5. customto remove low-boiling point ingredients
6. additionMethanol was added to the residue
7. filtrationthe deposited solid was collected by filtration
8. customThe thus-obtained crude product
9. customwas purified by silica gel column chromatography
10. additionmixed solvent as a developing solvent
11. customto give