反应详情

To a mixture of 2-fluoro-5-(trifluoromethoxy)aniline (2 g, 10 mmol) dissolved in DMF (4 mL) was slowly added a solution of N-bromosuccinimide (2.2 g, 12 mmol) dissolved in DMF (5 mL). The reaction mixture was stirred at RT for 1 h, concentrated and extracted with ethyl acetate/water. The organic layer was washed with brine, partitioned, dried over sodium sulfate, filtered, concentrated, and purified by silica chromatography (100% hexanes) to produce the title intermediate as a red oil (2 g, 70% yield). (m/z): [M+H]+ calcd for C7H4BrF4NO 273.94; 275.94. found 276.2.

1. concentrationconcentrated
2. extractionextracted with ethyl acetate/water
3. washThe organic layer was washed with brine
4. custompartitioned
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified by silica chromatography (100% hexanes)