反应详情

To a solution of (4-fluoro-3-methoxyphenyl)(3-fluoro-5-(1,1,2,2-tetrafluoroethoxy)phenyl)methanone (16 g, 43 mmol) in THF (70 mL) was added Ti(OEt)4 (15 g, 65.9 mmol), followed by the addition of (R)-2-methylpropane-2-sulfinamide (5.86 g, 48.3 mmol). The reaction mixture was heated at reflux for 16 h, allowed to cool to room temperature and quenched by addition of saturated NaCl. The resulting mixture was filtered and the organic solvent was removed under reduced pressure. The residue was purified by ISCO chromatography using hexanes/EtOAc (10-50%) to afford (R)-N-((4-fluoro-3-methoxyphenyl)(3-fluoro-5-(1,1,2,2-tetrafluoroethoxy)phenyl)methylene)-2-methylpropane-2-sulfinamide as an oil (15 g, 75%). LCMS: RT=4.01 min, [M+H] 468.1 (Phenomenex Luna C18 column, 4.6×50 mm eluting with 10-90% MeOH/H2O over 4 minutes containing 0.1% TFA; 4 mL/min, monitoring at 220 nm).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 16 h
3. customquenched by addition of saturated NaCl
4. filtrationThe resulting mixture was filtered
5. customthe organic solvent was removed under reduced pressure
6. customThe residue was purified by ISCO chromatography