反应详情

To a solution of 66.62A (0.39 g, 1.1 mmol) in DMF (5 mL), was added NaH (0.034 g, 1.4 mmol). The mixture was stirred at room temperature for 10 minutes and then iodomethane (0.20 mL, 3.2 mmol) was added. The mixture was stirred at room temperature for 60 minutes and then it was diluted with EtOAc, washed with water and brine, and dried over anhydrous Na2SO4. After removing solvent, the residue was purified by flash chromatography (silica gel, 1:9 EtOAc/hexane) and gave 66.62B, colorless oil, in 64% yield (260 mg).

1. stirringThe mixture was stirred at room temperature for 60 minutes
2. washwashed with water and brine
3. dry with materialdried over anhydrous Na2SO4
4. customAfter removing solvent
5. customthe residue was purified by flash chromatography (silica gel, 1:9 EtOAc/hexane)