反应详情

A mixture of ethyl 4-hydroxybenzoate (0.46 g, 2.80 mmol), 1-iodo-4,4,4-trifluorobutane (0.67 g, 2.80 mmol) and anhydrous K2CO3 (1.16 g, 8.40 mmol) in methyl ethyl ketone (5 ml) was heated under reflux for 4 h under an atmosphere of argon. On cooling to room temperature, the solvent was removed under reduced pressure and the residue was partitioned between water (15 ml) and Et2O (30 ml). The organic layer was separated, and the aqueous phase extracted with Et2O (2×20 ml). The combined organic extracts were washed with brine (15 ml) and dried (Na2SO4). The solvent was removed under reduced pressure to give a solid which was purified by flash chromatography (3:1 Hexane/EtOAc) to give the title compound (0.67 g, 87%) as a colourless solid.

1. temperaturewas heated
2. temperatureunder reflux for 4 h under an atmosphere of argon
3. customthe solvent was removed under reduced pressure
4. customthe residue was partitioned between water (15 ml) and Et2O (30 ml)
5. customThe organic layer was separated
6. extractionthe aqueous phase extracted with Et2O (2×20 ml)
7. washThe combined organic extracts were washed with brine (15 ml)
8. dry with materialdried (Na2SO4)
9. customThe solvent was removed under reduced pressure
10. customto give a solid which
11. customwas purified by flash chromatography (3:1 Hexane/EtOAc)