N-bromobutanimide → 1,5-Dibromo-2,4-difluorobenzene

A total of 1.6 g of 1-bromo-2,4-difluorobenzene was suspended in 8.29 ml of sulfuric acid, and 1.62 g of N-bromosuccinimide was added under ice-cooling. After stirring at room temperature for 17 hours, the reaction mixture was poured onto ice-water and extracted with ethyl acetate. The resulting organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and brine, dried over magnesium sulfate and the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (hexane), to give 2.18 g of the title compound as a pale yellow oil.

1. temperaturecooling
2. additionthe reaction mixture was poured onto ice-water
3. extractionextracted with ethyl acetate
4. washThe resulting organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and brine
5. dry with materialdried over magnesium sulfate
6. customthe solvent was evaporated
7. customThe residue was purified
8. customseparated by silica gel column chromatography (hexane)

ORD record

ord-11047ceb60004de8b54b2d9cc71a3752

Source dataset

uspto-grants-2010_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07776890B2