反应详情

A mixture of methyl 2-(2-fluorophenylamino)-3,4-difluoro-5-((trimethylsilyl)ethynyl)benzoate (9 mmol, 3.5 g), HgSO4 (9 mmol, 2.67 g), and cone. H2SO4 (18 mmol, 0.96 ml) in acetone:H2O (70:12 ml) was refluxed at 65° C. overnight. The mixture was concentrated, diluted with EtOAc, and washed with water and brine. The organic fractions are combined, dried over MgSO4 and concentrated under reduced pressure. The crude material (brown solid) was triturated with MeOH and the precipitate was filtered, washed with additional MeOH and dried to yield the desired product in 60% (1.78 g).

1. concentrationThe mixture was concentrated
2. additiondiluted with EtOAc
3. washwashed with water and brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated under reduced pressure
6. customThe crude material (brown solid) was triturated with MeOH
7. filtrationthe precipitate was filtered
8. washwashed with additional MeOH
9. customdried