反应详情

温度

160 °C

To a mixture of 2-(2-ethyl-5-iodophenyl)cyclohexane-1,3-dione (0.250 g, 0.73 mmol), 4-chloro-2-fluorophenol (0.535 g, 3.65 mmol) and cesium carbonate (0.477 g, 1.46 mmol) is added powdered 3 Å molecular sieves (0.300 g) and copper (II) trifluoromethanesulfonate (0.012 g, 0.037 mmol). After degassing with nitrogen anhydrous toluene (4 ml) is added, and the suspension is heated at 160° C. for 1 hour under microwave irradiation. The reaction mixture is acidified with 2M aqueous hydrochloric acid and extracted with dichloromethane (×2). The organic phase is separated then evaporated under reduced pressure to yield a crude product which is purified by preparative reverse-phase HPLC to afford 2-[5-(4-chloro-2-fluoro-phenoxy)-2-ethylphenyl]cyclohexane-1,3-dione.

1. additionis added
2. customAfter degassing with nitrogen anhydrous toluene (4 ml)
3. additionis added
4. extractionextracted with dichloromethane (×2)
5. customThe organic phase is separated
6. customthen evaporated under reduced pressure
7. customto yield a crude product which
8. customis purified by preparative reverse-phase HPLC