反应 #61171

ord-73ecc3b717224c47a915a4cc25aca307

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩concentrated in vacuo
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in EtOAc (100 mL)
  3. 3
    洗涤washed with water (2×100 mL)
  4. 4
    干燥dried (Na2SO4)
  5. 5
    浓缩concentrated in vacuo
  6. 6
    其他Purification by silica gel column chromatography

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07427683B2uspto-grants-2008_09