反应详情

温度

105 °C

To a suspension of 2-fluoro-6-methoxy phenol (1) (2.8 g, 20 mmol), N,N-dimethyl glycine.HCl (837 mg, 6 mmol), Cs2CO3 (13 g, 40 mmol), 1-fluoro-4-iodobenzene (2.3 mL, 20 mmol), in Dioxane (40 ml) was added copper iodone (381 mg, 2 mmol). The reaction mixture was stirred at 105° C. over 1 week. Upon heating the reaction mixture turned from brown to a bright green. After cooling to room temperature, the reaction mixture was filtered and the filtrate was concentrated in-vacuo. The crude was purified by silica gel eluted with hexane/EtOAc (10:1), concentrated in-vacuo, to provide 300 g (21% yield) of product (2).

1. temperatureUpon heating the reaction mixture
2. temperatureAfter cooling to room temperature
3. filtrationthe reaction mixture was filtered
4. concentrationthe filtrate was concentrated in-vacuo
5. customThe crude was purified by silica gel
6. washeluted with hexane/EtOAc (10:1)
7. concentrationconcentrated in-vacuo