反应详情

To a mixture of 122a (598 mg, 2.0 mmol) in DMF (10 mL) was added NaH (64 mg, 1.6 mmol) at 0° C. and the mixture was stirred for 0.5 h. To the mixture was added iodomethane (227 mg, 1.6 mmol) in DMF dropwise at 0° C. The mixture was stirred for 0.5 h and quenched with water (20 mL). It was then extracted with dichloromethane (3×30 mL). The combined extract was concentrated under reduced pressure and the residue was purified with silica-gel column chromatography eluting with petroleum ether/ethyl acetate (5:1 to 2:1) to afford 122b (360 mg, 58%) as a light yellow solid. MS-ESI: [M+H]+ 311.1

1. stirringThe mixture was stirred for 0.5 h
2. customquenched with water (20 mL)
3. extractionIt was then extracted with dichloromethane (3×30 mL)
4. extractionThe combined extract
5. concentrationwas concentrated under reduced pressure
6. customthe residue was purified with silica-gel column chromatography
7. washeluting with petroleum ether/ethyl acetate (5:1 to 2:1)