反应详情

A suspension of 8-bromo-1-octene (1.00 g, 5.24 mmol), 4-[5-(5,5,6,6,7,7,8,8,8-nonafluorooctyloxy)-pyrimidin-2-yl]-phenol (2.54 g, 5.50 mmol) and cesium carbonate (3.40 g, 10.47 mmol) in acetone (40 ml) was heated under reflux for 12 h, cooled to room temperature, washed with water and the organic layer extracted into ethyl acetate/hexane (3 times). The combined organic extracts were washed with brine, dried (MgSO4) and the solvent removed in vacuo. The residues were purified by column chromatography [silica gel, eluted with hexane/ethyl acetate (9:1)] to yield a colorless solid, which was recrystallized from ethanol.

1. temperaturewas heated
2. temperatureunder reflux for 12 h
3. washwashed with water
4. extractionthe organic layer extracted into ethyl acetate/hexane (3 times)
5. washThe combined organic extracts were washed with brine
6. dry with materialdried (MgSO4)
7. customthe solvent removed in vacuo
8. customThe residues were purified by column chromatography [silica gel, eluted with hexane/ethyl acetate (9:1)]
9. customto yield a colorless solid, which
10. customwas recrystallized from ethanol