反应详情

A mixture of 2-(2-chlorophenylamino)-3,4-difluoro-6-trimethylsilanylethynylbenzoic acid methyl ester (1.00 g, 2.54 mmol), HgSO4 (761 mg, 2.54 mmol), and concentrated H2SO4 (0.27 mL) in acetone-water (22 mL/4 mL) was refluxed for 3 hours. The reaction mixture was concentrated in vacuo, diluted with EtOAc-THF, and washed with water and brine. The organic layer was dried over MgSO4, filtered, and concentrated to give the crude material that was purified by silica gel flash column chromatography (8% EtOAc in hexanes) to afford the desired product (496 mg, 58%).

1. temperaturewas refluxed for 3 hours
2. concentrationThe reaction mixture was concentrated in vacuo
3. additiondiluted with EtOAc-THF
4. washwashed with water and brine
5. dry with materialThe organic layer was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customto give the crude material that
9. customwas purified by silica gel flash column chromatography (8% EtOAc in hexanes)