反应详情

温度

70 °C

To a heterogeneous mixture of 20 (2.16 g, 6.90 mmol) in acetone (22 mL) were sequentially added 1-bromo-2-chloroethane (7.2 mL, 86.50 mmol) and potassium carbonate (3.00 g, 21.71 mmol). The reaction was stirred and heated at 70° C. for 17 hours before it was allowed to cool to room temperature and was filtered. The solids were rinsed with a 3:1 mixture of dichloromethane/methanol (25 mL×3), and the filtrate was isolated and evaporated to give the crude product. Column chromatography on silica (dichloromethane to 20/1 to 15/1 to 5/1dichloromethane/methanol) gave 21 as a pale yellow solid (0.96 g, 35.5%).

1. temperatureto cool to room temperature
2. filtrationwas filtered
3. washThe solids were rinsed with a 3:1 mixture of dichloromethane/methanol (25 mL×3)
4. customthe filtrate was isolated
5. customevaporated
6. customto give the crude product