反应详情

温度

80 °C

To 2.8 mmol 4-cyclobutanesulfonyl-1,2-difluoro-benzene in 20 ml N,N-dimethylacetamide was added 8.3 mmol piperazine, and the mixture was heated at 80° C. for 45 min. The mixture was then concentrated in vacuo, and the residue was chromatographed on silica gel (eluant: ethyl acetate/methanol gradient). The product-containing fractions were combined and concentrated in vacuo. The residue was resuspended in 100 ml dioxane, and 6.0 mmol HCl (as a 4 M solution in dioxane) was added. After stirring for 10 min, the ensuing white crystals were collected by filtration, washing twice with ether, to afford the title compound.

1. concentrationThe mixture was then concentrated in vacuo
2. customthe residue was chromatographed on silica gel (eluant: ethyl acetate/methanol gradient)
3. concentrationconcentrated in vacuo
4. filtrationthe ensuing white crystals were collected by filtration
5. washwashing twice with ether