反应详情

A solution of 3-phenyl-1H-pyrazole (4.08 g, 28.3 mmol) and NBS (5.04 g, 28.3 mmol) in DMF (40 mL) was stirred for 1 h at room temperature. The reaction mixture was poured into water and extracted with AcOEt. The extract was washed with water and brine, dried over MgSO4, and concentrated under reduced pressure. The residue was recrystallized from hexane/AcOEt to give the title compound (5.84 g, 93% yield) as a white solid: mp 114-116° C.; NMR (300 MHz, CDCl3): δ ppm 7.39-7.50 (31-1, m), 7.64 (1H, s), 7.77 (2H, d, J=6.8 Hz), 10.73 (1H, brs).

1. extractionextracted with AcOEt
2. washThe extract was washed with water and brine
3. dry with materialdried over MgSO4
4. concentrationconcentrated under reduced pressure
5. customThe residue was recrystallized from hexane/AcOEt