反应详情

n-Butyllithium (0.229 mL, 0.57 mmol) was added to 6-bromo-3-methoxy-2,4-dimethylpyridine (124 mg, 0.57 mmol) in THF (7 mL) at −78° C. under nitrogen atmosphere. The reaction was stirred for 30 min before (E)-N-((2-bromopyridin-4-yl)(2-cyano-3-fluorophenyl)methylene)-2-methylpropane-2-sulfinamide (180 mg, 0.44 mmol) in THF (2 mL) was added. The reaction was kept at −78° C. for 1 hour and then allowed to reach room temp. Methanol (5 mL) was added followed by hydrochloric acid in diethylether (1.323 mL, 1.32 mmol) and the reaction mixture was stirred 1 hour at room temperature. NaHCO3(sat) was added and the mixture was extracted with EtOAc (×2). The combined organic phases were dried and concentrated to give the title compound (200 mg, 97%), which was used without further purification. MS (ES+) m/z 441, 443 [M+1]+.

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