反应详情

N-(3-Acetyl-5-pentafluorosulfanylphenyl)-2,2,2-trifluoroacetamide (20 mg) was initially introduced dissolved in glacial acetic acid (1 ml), and bromine (9 mg) dissolved in glacial acetic acid (90 μl) was slowly added dropwise. After stirring at RT for 30 min, the mixture was warmed at 60° C. for 1 h. After cooling to RT, the glacial acetic acid was diluted with a large quantity of water and extracted three times with ethyl acetate. The combined extracts were washed with sodium hydrogencarbonate solution until acid-free, dried over magnesium sulfate, filtered and concentrated. The crude product obtained (24 mg) was employed in the next stage without further purification.

1. additionwas slowly added dropwise
2. temperaturethe mixture was warmed at 60° C. for 1 h
3. temperatureAfter cooling to RT
4. extractionextracted three times with ethyl acetate
5. washThe combined extracts were washed with sodium hydrogencarbonate solution until acid-free,
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated