954137-48-5

112486-09-6

954137-48-5

The general procedure for the synthesis of 5-bromo-7,7-dimethylbenzo[c]fluorene from 7,7-dimethyl-7H-benzo[c]fluorene was as follows: 7,7-dimethyl-7H-benzo[c]fluorene (38.2 g, 156 mmol) was dissolved in 300 mL of chloroform and the solution was cooled down to 0 °C. A chloroform solution of bromine (117 g, 660 mmol) was slowly added dropwise under stirring conditions, with the rate of dropwise acceleration controlled to ensure that the reaction temperature did not exceed 5 °C. After the reaction mixture was kept cool in an ice bath, it was gradually warmed to room temperature and stirred overnight. Upon completion of the reaction, the reaction was quenched by the addition of 200 mL of 10% sodium thiosulfate solution and the organic and aqueous phases were separated. The aqueous phase was extracted with dichloromethane (DCM) several times. The organic phases were combined, washed with distilled water, dried and concentrated to remove the solvent. The resulting solid was recrystallized by mixed toluene/heptane solvent to give 50 g of colorless solid product in 99% yield of the theoretical value.