反应详情

To a solution of 1-(1-methyl-1H-pyrazol-4-yl)ethanone (0.602 g, 4.85 mmol) in chloroform (20 mL) and of 33% HBr in acetic acid (3.92 mg, 0.05 mmol) was added dropwise a chloroform solution containing Br2 (0.262 mL, 5.09 mmol) via an addition funnel. The reaction mixture was stirred at room temperature for 1 h and then concentrated under reduced pressure. The crude solid was triturated in ethyl acetate, filtered, washed and dried in vacuo. The free base was obtained by triturating the product in 5% NaHCO3 for 2 h. The solid that formed were collected by filtration, washed with water and isopropyl alcohol and then dried in vacuo. Isolation gave 874 mg of the title compound.

1. concentrationconcentrated under reduced pressure
2. customThe crude solid was triturated in ethyl acetate
3. filtrationfiltered
4. washwashed
5. customdried in vacuo
6. customThe free base was obtained
7. customby triturating the product in 5% NaHCO3 for 2 h
8. customThe solid that formed
9. filtrationwere collected by filtration
10. washwashed with water and isopropyl alcohol
11. customdried in vacuo