反应详情

温度

80 °C

To the 3-methoxy-6-methyl-2-(3-trifluoromethyl-phenyl)-pyridine synthesized above (1.3 g, 4.86 mmol) and NBS (1.04 g, 5.83 mmol) in CCl4 (25 mL) was added benzoyl peroxide (0.12 g, 0.49 mmol). The reaction was stirred at 80° C. under N2 for 20 h. The reaction was cooled to room temperature and concentrated. The residue was dissolved in mixture of dichloromethane and hexanes (1:1, 8 mL) and purified by silica gel column chromatography using 1:1 dichloromethane-hexanes to afford 0.74 g (44%) of 6-bromomethyl-3-methoxy-2-(3-trifluoromethyl-phenyl)-pyridine as off-white solid.

1. temperatureThe reaction was cooled to room temperature
2. concentrationconcentrated
3. dissolutionThe residue was dissolved in mixture of dichloromethane and hexanes (1:1, 8 mL)
4. custompurified by silica gel column chromatography