反应详情

Methylmagnesium bromide (3 M in ether, 0.45 mL, 1.33 mmol) was added at 0° C. to a solution of 331c) (0.36 g, 0.89 mmol) in THF (70 mL) and the resulting mixture was stirred at this temperature for 6 h. The mixture was quenched with ammonium chloride solution (20 mL) and extracted with ethyl acetate (2×50 mL). The organic phase was washed with brine, dried over sodium sulfate and evaporated. The residue was purified by flash column chromatography [silica; dichloromethane with 0-1.5% methanol]. Light yellow solid. Yield: 0.22 g (59% of theory)

1. customThe mixture was quenched with ammonium chloride solution (20 mL)
2. extractionextracted with ethyl acetate (2×50 mL)
3. washThe organic phase was washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated
6. customThe residue was purified by flash column chromatography [silica; dichloromethane with 0-1.5% methanol]