反应详情

Hydrogen peroxide (8.096 ml) was added dropwise to the well stirred solution of 3-oxo-N-[4-(trifluoromethyl)phenyl]butanamide (10 g) [obtained from above step-a], potassium bromide (4.85 g) and conc. HCl (7.446 ml) in toluene (100 ml) at room temperature. Reaction was monitored by TLC. D.M water was added to the reaction mixture and organic layer was separated. Aqueous layer was extracted with ethyl acetate (50 ml×2). Combined organic layer was washed with brine, dried over sodium sulfate and concentrated to give crude compound. The crude was purified by column chromatography to give pure 2-bromo-3-oxo-N-[4-(trifluoromethyl)phenyl]butanamide (6.4 g).

1. customReaction
2. customwas separated
3. extractionAqueous layer was extracted with ethyl acetate (50 ml×2)
4. washCombined organic layer was washed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customto give crude compound
8. customThe crude was purified by column chromatography