反应详情

温度

170 °C

To a mixture of 2-(5-bromo-2-ethylphenyl)-5,5-dimethylcyclohexane-1,3-dione (0.236 g, 0.73 mmol), cesium carbonate (0.477 g, 1.46 mmol), 4-chloro-3-fluorophenol (0.535 g, 3.65 mmol), copper (II) trifluoromethanesulfonate (0.012 g, 0.04 mmol) and powdered 3 Å molecular sieves (0.300 g) is added anhydrous toluene (4 ml). After purging with nitrogen the reaction mixture is heated at 170° C. for 1 hour under microwave irradiation, then allowed to cool to room temperature. After quenching with 2M aqueous hydrochloric acid the crude product is extracted into dichloromethane (×2) and the phases are separated. Organic solvents are removed in vacuo and the crude product is purified by preparative reverse-phase HPLC to afford 2-[5-(4-chloro-3-fluorophenoxy)-2-ethylphenyl]-5,5-dimethylcyclohexane-1,3-dione as a white solid.

1. customAfter purging with nitrogen the reaction mixture
2. temperatureto cool to room temperature
3. customAfter quenching with 2M aqueous hydrochloric acid the crude product
4. extractionis extracted into dichloromethane (×2)
5. customthe phases are separated
6. customOrganic solvents are removed in vacuo
7. customthe crude product is purified by preparative reverse-phase HPLC