反应详情

To a solution of 2,4-difluoronitrobenzene (2.09 g, 13.1 mmol) in EtOH (10 mL) at ambient temperature was added piperidine (3.35 g, 39.4 mmol) dropwise. The reaction was allowed to stir overnight and concentrated in vacuo. The residue was dissolved in EtOAc (100 mL), washed with water (2×100 mL), dried (Na2SO4) and concentrated in vacuo. Purification by silica gel column chromatography afforded 1.10 (37%) of the title compound as an oil. Mass spectrum (ESI, m/z): Calcd. for C11H13FN2O2, 225.1 (M+H), found 225.1.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in EtOAc (100 mL)
3. washwashed with water (2×100 mL)
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customPurification by silica gel column chromatography