反应详情

温度

60 °C

To a solution of the product from Step A (75.4 mmol) in 100 mL of DMF was added potassium carbonate (20.8 g, 150.7 mmol), followed by allyl bromide (11.7 mL, 135 mmol). The reaction was warmed to 60° C. and stirred for one hour. The solution was poured into EtOAc and washed with water, saturated NaHCO3 solution and brine, dried (Na2SO4), filtered, and concentrated in vacuo. The resulting product was purified by silica gel chromatography (20-30% EtOAc/hexane) to provide the titled product, along with unreacted starting material (4.39 g, 26%).

1. washwashed with water, saturated NaHCO3 solution and brine
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe resulting product was purified by silica gel chromatography (20-30% EtOAc/hexane)