反应详情

To an ice-cold solution of 3-bromo-5-nitro-phenol (21.0 g, 96.33 mmol) in acetone (420.0 mL) was added K2CO3 (40.0 g, 289.41 mmol) followed by addition of benzyl bromide (17.20 mL, 144.40 mmol). The resulting reaction mixture was stirred at room temperature for 2 h. The reaction mixture was then diluted with water and extracted with EtOAc (3×250.0 mL). The combined organics was dried over anhydrous Na2SO4 and concentrated under reduced pressure. The crude was purified over silica gel (100-200 M, 5% EtOAc-Hexane) to get the desired product (27.0 g, 91%).

1. customThe resulting reaction mixture
2. extractionextracted with EtOAc (3×250.0 mL)
3. dry with materialThe combined organics was dried over anhydrous Na2SO4
4. concentrationconcentrated under reduced pressure
5. customThe crude was purified over silica gel (100-200 M, 5% EtOAc-Hexane)