反应详情

温度

0 °C

A solution of rac-N-[1-(3-bromo-phenyl)-1-(1H-pyrazol-3-yl)-ethyl]-2-chloro-acetamide (1.22 g, 3.56 mmol) in THF (40 mL) was added dropwise to a suspension of sodium hydride (0.28 g, 7.12 mmol) in THF (40 mL) at 0° C. under nitrogen. The mixture was stirred at 0° C. for 1 hour. The mixture was diluted with water and the product extracted with DCM. The organic layer was separated, dried (MgSO4), filtered and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica gel; AcOEt in DCM 50/50 to 100/0). The desired fractions were collected and concentrated in vacuo to yield rac-4-(3-bromo-phenyl)-4-methyl-4,5-dihydro-pyrazolo[1,5-a]pyrazin-6-one (0.7 g, 64% yield) as a white solid.

1. extractionthe product extracted with DCM
2. customThe organic layer was separated
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customthe solvents evaporated in vacuo
6. customThe crude product was purified by flash column chromatography (silica gel; AcOEt in DCM 50/50 to 100/0)
7. customThe desired fractions were collected
8. concentrationconcentrated in vacuo