反应详情

The title compound was prepared essentially as in Example 1 by combining 5-octyl-2-(4-hydroxyphenyl)pyrimidine (2.0 g, 7.3 mmol), 3-(2-(2-(pentafluoroethoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)-1-bromopropane (3.38 g, 7.47 mmol; prepared by combining 1,3-dibromopropane with 3-(2-(2-(pentafluoroethoxy)tetrafluorooethoxy)-2,2-difluoroethanol), and potassium carbonate (1.16 g, 8.43 mmol) in acetonitrile (20 mL) and refluxing the resulting mixture under nitrogen overnight. The mixture was cooled and filtered, and the resulting solids were washed with toluene (50 mL). The toluene was then removed under reduced pressure, and the resulting waxy solid was dissolved in toluene (50 mL) and washed with three 30 mL aliquots of perfluorohexane. After removing the toluene under reduced pressure, the resulting crude product was further purified by silica gel chromatography, eluting with 20 volume percent ethyl acetate/hexane, to yield 3.60 g of purified product.

1. customprepared
2. temperaturerefluxing the resulting mixture under nitrogen overnight
3. temperatureThe mixture was cooled
4. filtrationfiltered
5. washthe resulting solids were washed with toluene (50 mL)
6. customThe toluene was then removed under reduced pressure
7. dissolutionthe resulting waxy solid was dissolved in toluene (50 mL)
8. washwashed with three 30 mL aliquots of perfluorohexane
9. customAfter removing the toluene under reduced pressure
10. customthe resulting crude product was further purified by silica gel chromatography
11. washeluting with 20 volume percent ethyl acetate/hexane