The general procedure for the synthesis of 2,6-dichloro-3-bromotoluene from 2,6-dichlorotoluene was as follows: 2,6-dichlorotoluene (50.0 g, 0.31 mol), iodine (0.10 g, 0.39 mmol), and 325-mesh iron powder (0.70 g, 12.5 mmol) were dissolved in carbon tetrachloride (60 mL), and bromine (52.8 g, 0.33 mol) was added slowly dropwise. mol), and the dropwise addition process was controlled to be completed within 20 min. The reaction mixture was stirred at room temperature for 3 hours. After completion of the reaction, the mixture was poured into ice water and extracted with 1,2-dichloroethane. The organic layer was washed with saturated sodium bisulfite solution and dried with anhydrous sodium sulfate. Finally, the solvent was removed by distillation under reduced pressure to give 1-bromo-2,4-dichloro-3-methylbenzene (76.01 g, 100% yield).
