反应详情

To a mixture of 11.6 g of 1-[2-amino-4-(trifluoromethyl)phenyl]ethanone, 60 mL of acetonitrile, and 230 mL of diethyl ether was added 2.85 g of Amberlyst (registered trademark) 15, and 10.1 g of N-bromosuccinimide was added thereto in three times in an ice bath. After stirring for 30 minutes in an ice bath, the mixture was stirred at room temperature overnight. The insoluble material was filtered and washed with ethyl acetate. To the filtrate were added water and ethyl acetate, and the aqueous layer was separated. The organic layer was washed with a 10% aqueous sodium thiosulfate solution and saturated brine, and dried over anhydrous magnesium sulfate, and then solvent was evaporated. The residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to obtain 10.36 g of 1[2-amino-5-bromo-4-(trifluoromethyl)phenyl]ethanone.

1. additionwas added
2. stirringthe mixture was stirred at room temperature overnight
3. filtrationThe insoluble material was filtered
4. washwashed with ethyl acetate
5. additionTo the filtrate were added water and ethyl acetate
6. customthe aqueous layer was separated
7. washThe organic layer was washed with a 10% aqueous sodium thiosulfate solution and saturated brine
8. dry with materialdried over anhydrous magnesium sulfate
9. customsolvent was evaporated
10. customThe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate)