反应详情

To a solution of 5.08 g (10.7 mmol) crude 2b in 50 ml ml pyridine was added 4.37 g (42.8 mmol) acetic acid anhydride. The reaction mixture was stirred over night and poured into ice-cold ethyl acetate. The organic phase was washed with water, diluted aqueous sodium hydrogen sulfate, water and brine and were dried with magnesium sulfate. The crude product was purified by silica column chromatography (ethyl acetate:hexane gradient 1:8→1:4). The desired product 2c was obtained in 79% yield (4.36 g, 8.45 mmol).

1. additionpoured into ice-cold ethyl acetate
2. washThe organic phase was washed with water, diluted aqueous sodium hydrogen sulfate, water and brine
3. dry with materialwere dried with magnesium sulfate
4. customThe crude product was purified by silica column chromatography (ethyl acetate:hexane gradient 1:8→1:4)