反应详情

A solution of 20.0 g of 1-isopropyl-4-methoxy benzene, 1.07 g of ammonium nitrate, and 23.7 g of N-bromosuccinimide in MeCN (66.5 ml) was stirred at room temperature for one hour. To the reaction solution was added EtOAc and a saturated aqueous solution of NaHCO3, liquid separation was performed, and the aqueous layer was extracted with EtOAc. The combined organic layer was washed with saturated brine and dried over MgSO4, then, the drying agent was separated by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (silicagel 60; mobile phase: EtOAc/n-hexane=1/9, v/v) to obtain 30.4 g of the title compound.

1. customa saturated aqueous solution of NaHCO3, liquid separation
2. extractionthe aqueous layer was extracted with EtOAc
3. washThe combined organic layer was washed with saturated brine
4. dry with materialdried over MgSO4
5. customthe drying agent was separated by filtration
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe residue was purified by column chromatography (silicagel 60; mobile phase: EtOAc/n-hexane=1/9, v/v)