反应详情

n-Butyllithium (1.174 mL, 2.94 mmol) was added to 4-bromo-2-(difluoromethyl)-6-methylpyridine (543 mg, 2.45 mmol) in THF (15 mL) at −78° C. under nitrogen atmosphere. The reaction was stirred for 30 min before (E)-N-((2-chloropyridin-4-yl)(2-cyano-3-fluorophenyl)methylene)-2-methylpropane-2-sulfinamide (890 mg, 2.45 mmol) in THF (5 mL) was added. The reaction was kept at −78° C. for 1 hour and then allowed to reach room temperature. MeOH (15 mL) was added followed by hydrochloric acid in diethylether (7.34 mL, 7.34 mmol) and the reaction was stirred for 1 hour. NaHCO3(sat) was added and the mixture was extracted with EtOAc (×2). The combined organic phases were dried and concentrated to give 0.5 g (51%) of the title compound, which was used without further purification. MS (ES+) m/z 403 [M+1]+.

1. additionwas added
2. customto reach room temperature
3. extractionthe mixture was extracted with EtOAc (×2)
4. customThe combined organic phases were dried
5. concentrationconcentrated