反应详情

To a mixture of 127a (480 mg, 2.0 mmol) in anhydrous DMF (10 mL) was added NaH (purity 60%) (64 mg, 1.6 mmol) at 0° C. and the resulting mixture was stirred for 0.5 h. To the mixture was added iodomethane (227 mg, 1.6 mmol) in DMF (5 mL) dropwise at 0° C. The reaction mixture was stirred for additional 1.5 h and quenched with water (20 mL). It was then extracted with dichloromethane (3×20 mL) and the combined organic layer was evaporated under reduced pressure. The residue was purified by reverse-phase Combiflush (A: 2% aqueous NH4HCO3, B: acetonitrile) to afford 127b (120 mg, 24%) as a light yellow solid. MS-ESI: [M+H]+ 254.3

1. stirringThe reaction mixture was stirred for additional 1.5 h
2. customquenched with water (20 mL)
3. extractionIt was then extracted with dichloromethane (3×20 mL)
4. customthe combined organic layer was evaporated under reduced pressure
5. customThe residue was purified by reverse-phase Combiflush (A: 2% aqueous NH4HCO3, B