反应详情

温度

60 °C

A mixture of (4-chloro-2-ethynylphenoxy)acetic acid (Intermediate 238; 211 mg; 1.00 mmol), 6-bromo-2-tert-butyl-1,2-benzisothiazol-3(2H)-one-1,1-dioxide (prepared as described in Tetrahedron, 2006, 62, 7902-7910, 382 mg; 1.20 mmol), dichlorobis(triphenylphosphine)palladium(II) (70 mg; 0.10 mmol) and cuprous iodide (9.5 mg; 0.05 mmol) in anhydrous THF (4 ml) was degassed for 10 minutes then treated with triethylamine (1.00 ml; 7.21 mmol) and the mixture stirred at 60° C. for 16 h. EtOAc was added and the organic phase washed with a sat. NH4Cl solution then brine. The organic phase was dried on MgSO4, filtered and concentrated under reduced pressure to give a residue which was purified by preparative HPLC to afford the title compound as a white solid.

1. customwas degassed for 10 minutes
2. washthe organic phase washed with a sat. NH4Cl solution
3. customThe organic phase was dried on MgSO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customto give a residue which
7. customwas purified by preparative HPLC