反应详情

First, into a 200-mL three-neck flask were placed 2.2 g (6.0 mmol) of 2-(4-bromophenyl)-3-phenylquinoxaline, 1.9 g (6.0 mmol) of 3,6-diphenyl-9H-carbazole, and 1.1 g (12.0 mmol) of sodium tert-butoxide. The air in the flask was replaced with nitrogen, and 60 mL of xylene was placed into this flask. The mixture was degassed by stirring under reduced pressure. To this mixture were added 0.2 mL of tri(tert-butyl)phosphine and 71 mg (0.12 mmol) of bis(benzylideneacetone)palladium(0). This mixture was stirred under a nitrogen stream at 140° C. for 6 hours. After the predetermined time had elapsed, water was added to the obtained mixture, and the mixture was separated into an organic layer and an aqueous layer. Organic substances were extracted with toluene from the aqueous layer. The solution of the obtained extract was combined with the organic layer, and the mixture was washed with saturated brine and dried with magnesium sulfate. The obtained mixture was gravity filtered, and the filtrate was concentrated to give an oily substance. This oily substance was purified by silica gel column chromatography (with a developing solvent of toluene), followed by recrystallization from toluene, whereby 3.0 g of a yellow powder of Cz1PQ-III, which is the substance to be produced, was obtained in 81% yield.

1. customFirst, into a 200-mL three-neck flask were placed
2. customwas placed into this flask
3. customThe mixture was degassed
4. stirringThis mixture was stirred under a nitrogen stream at 140° C. for 6 hours
5. customthe mixture was separated into an organic layer
6. extractionOrganic substances were extracted with toluene from the aqueous layer
7. extractionThe solution of the obtained extract
8. washthe mixture was washed with saturated brine
9. dry with materialdried with magnesium sulfate
10. filtrationfiltered
11. concentrationthe filtrate was concentrated
12. customto give an oily substance
13. customThis oily substance was purified by silica gel column chromatography (with a developing solvent of toluene),
14. customfollowed by recrystallization from toluene, whereby 3.0 g of a yellow powder of Cz1PQ-III, which
15. customto be produced
16. customwas obtained in 81% yield