反应详情

温度

50 °C

A solution of (2-bromo-4-chlorophenoxy)acetic acid (200 mg; 0.75 mmol, Intermediate 4) and 2-ethynylanisole (Aldrich, 107 μL; 0.83 mmol) in anhydrous, degassed ACN (2 mL) was treated with dichlorobis(triphenylphosphine)palladium(II) (38 mg; 0.05 mmol) followed after 5 minutes by copper iodide (10 mg; 0.05 mmol) and triethylamine (0.45 mL; 3.3 mmol). The reaction mixture was heated at 50° C. under stirring for 16 hours. The solvents were removed under vacuum, the residue was then taken up in EtOAc and washed with HCl (1N aqueous solution), the organic phase was washed with water (750 mL) then with brine (750 mL), dried over MgSO4, filtered and concentrated under vacuum to give a brown oily residue which was purified by preparative HPLC to afford the title compound as a brown oil.

1. customThe solvents were removed under vacuum
2. washwashed with HCl (1N aqueous solution)
3. washthe organic phase was washed with water (750 mL)
4. dry with materialwith brine (750 mL), dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customto give a brown oily residue which
8. customwas purified by preparative HPLC