反应详情

温度

80 °C

Then, 1.0 g of 4-chloro-6-phenylpyrimidine obtained in Step 1, 2.0 g of 3′-(dibenzothiophen-4-yl)-3-biphenylboronic acid, 5.3 mL of a 2M aqueous solution of potassium carbonate, 24 mL of toluene, and 3.0 mL of ethanol were put into a 100-mL three-neck flask equipped with a reflux pipe. Degasification by stirring under a reduced pressure was performed and the air in the flask was replaced with nitrogen. To this mixture, 61 mg of tetrakis(triphenylphosphine)palladium(0) (abbreviation: Pd(PPh3)4) was added and the mixture was heated at 80° C. for 7 hours to cause a reaction. An organic layer was extracted from the obtained mixture with the use of toluene and was washed with water and a saturated aqueous solution of sodium chloride. Anhydrous magnesium sulfate was added and gravity filtration was performed. After the solvent in this solution was distilled off, the obtained residue was dissolved in hot toluene and subjected to hot filtration through a filter aid in which Celite, alumina, Celite, Florisil, and Celite were stacked in this order. The solvent was distilled off and the obtained solid was recrystallized with toluene, so that 1.9 g of a white solid was obtained in a yield of 71%. Synthesis Scheme (D-2) of Step 2 is shown below.

1. customequipped with a reflux pipe
2. customDegasification
3. additionTo this mixture, 61 mg of tetrakis(triphenylphosphine)palladium(0) (abbreviation: Pd(PPh3)4) was added
4. customa reaction
5. extractionAn organic layer was extracted from the obtained mixture with the use of toluene
6. washwas washed with water
7. additionAnhydrous magnesium sulfate was added
8. filtrationgravity filtration
9. distillationAfter the solvent in this solution was distilled off
10. dissolutionthe obtained residue was dissolved in hot toluene
11. filtrationsubjected to hot filtration through a filter aid in which Celite, alumina, Celite, Florisil, and Celite
12. distillationThe solvent was distilled off
13. customthe obtained solid was recrystallized with toluene, so that 1.9 g of a white solid
14. customwas obtained in a yield of 71%
15. customSynthesis Scheme (D-2) of Step 2