反应详情

tert-Butyllithium (3.68 mL, 5.89 mmol) was added dropwise to THF (10 mL) at −100° C. under an argon atmosphere. A solution of 4-bromo-1-fluoro-2-methoxybenzene (0.604 g, 2.95 mmol) in THF (5 ml) was added dropwise followed by the addition of (E)-N-((3-bromophenyl)(2-cyano-3-fluorophenyl)methylene)-2-methylpropane-2-sulfinamide (1 g, 2.46 mmol) in THF (5 ml). The resulting reaction mixture was left on the thawing cooling bath for 30 min then the cooling bath was removed and the mixture was stirred at r.t. for 1 h. Hydrogen chloride-methanol solution (11.78 mL, 14.73 mmol) was added and the resulting mixture was stirred at r.t. for 1 h. The mixture was concentrated and purified on a silica gel column eluting with 0-10% 0.1 M NH3 in MeOH in DCM to afford 0.98 g (93%) of the title compound. MS (ES+) m/z 429, 431 (M+H)+

1. customThe resulting reaction mixture
2. waitwas left on the thawing
3. temperaturecooling bath for 30 min
4. customthe cooling bath was removed
5. stirringthe resulting mixture was stirred at r.t. for 1 h
6. concentrationThe mixture was concentrated
7. custompurified on a silica gel column
8. washeluting with 0-10% 0.1 M NH3 in MeOH in DCM