反应详情

To a solution of the material from Step 2 (500 mg, 2.18 mmol) in 8 mL of DMF was added iodomethane (0.68 mL, 10.9 mmol) and NaH (60% in oil, 131 mg, 3.28 mmol). The mixture was stirred at room temperature for 2 h. The reaction was quenched with water, and extracted with EtOAc and hexane. The organic layer was separated, washed with saturated sodium bicarbonate, dried over MgSO4, and concentrated. The crude was purified by flash silica column (eluting with 5% EtOAc in hexane) to get 1-bromo-4-(1-methoxy-2-methylpropan-2-yl)benzene (460 mg, 87%).

1. customThe reaction was quenched with water
2. extractionextracted with EtOAc and hexane
3. customThe organic layer was separated
4. washwashed with saturated sodium bicarbonate
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. customThe crude was purified by flash silica column (eluting with 5% EtOAc in hexane)