反应详情

温度

2.5 °C

339 g (679.7) mmol of 3,3′,4,4′-tetra(2-methylbutyloxy)biphenyl were dissolved in 800 ml of ethyl acetate. 120.98 g (679.7 mmol) of N-bromosuccinimide were then added in solid form over a period of 15 minutes under protective gas, in the absence of light and with cooling to 0-5° C. The suspension was slowly warmed to room temperature under a blanket of protective gas and was then stirred vigorously at room temperature for 4 hours. 500 ml of ethyl acetate and 300 ml of water were added, the phases were separated and the aqueous phase was extracted twice with 100 ml each time of ethyl acetate. The combined organic phases were washed twice with 50 ml each time of water and dried over MgSO4. The oil obtained was filtered through silica gel with the aid of hexane. Taking off the solvent gave 361.2 g (625.3 mmol, 92%) of 2-bromo-4,5,3′,4′-tetra(2-methylbutyloxy)biphenyl as a colorless oil.

1. temperatureThe suspension was slowly warmed to room temperature under a blanket of protective gas
2. customthe phases were separated
3. extractionthe aqueous phase was extracted twice with 100 ml each time of ethyl acetate
4. washThe combined organic phases were washed twice with 50 ml each time of water
5. dry with materialdried over MgSO4
6. customThe oil obtained
7. filtrationwas filtered through silica gel with the aid of hexane