反应详情

To a solution of 110 mg (0.52 mmol) (4-hydroxy-2-methyl-phenoxy)-acetic acid ethyl ester (WO02092590) and 169 mg (0.52 mmol) methanesulfonic acid 5-(4-trifluoromethoxy-phenyl)-pent-4-ynyl ester (example 1G]) in 5 ml acetonitrile were added 15.7 mg (0.10 mmol) NaI and 188 mg (0.58 mmol) Cs2CO3. The mixture was stirred at room temperature for 2 days and for 4.75 h at reflux. After filtration, the solvent was evaporated. The residue was redissolved in dichloromethane, dried (Na2SO4), filtered and evaporated. Purification by flash chromatography (SiO2, n-heptane/EtOAc 95:5) yielded 143 mg of the title compound as light yellow oil.

1. temperatureat reflux
2. filtrationAfter filtration
3. customthe solvent was evaporated
4. dissolutionThe residue was redissolved in dichloromethane
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customevaporated
8. customPurification by flash chromatography (SiO2, n-heptane/EtOAc 95:5)