反应 #2460344

ord-254a027671a3447a82dc3d9b7ac841be

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度heated
  2. 2
    温度under reflux for 2 hours
  3. 3
    其他the solvent was removed in vacuo
  4. 4
    workup.DISSOLUTIONthe residue dissolved in ethyl acetate
  5. 5
    萃取The mixture was extracted (×3) with ethyl acetate
  6. 6
    洗涤washed with water and saturated aqueous sodium chloride solution
  7. 7
    干燥before drying over magnesium sulfate
  8. 8
    其他Evaporation of the solvent

实验过程

4Methoxy-3-nitropyridine hydrochloride (11.2 g, 58.9 mmol) in ethanol (75 ml) was treated with a 70% solution of ethylamine in water (64 ml) and heated under reflux for 2 hours. After cooling to room temperature, the solvent was removed in vacuo and the residue dissolved in ethyl acetate and water. The mixture was extracted (×3) with ethyl acetate, washed with water and saturated aqueous sodium chloride solution before drying over magnesium sulfate. Evaporation of the solvent afforded the title compound (11.7 g, 96%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07459454B2uspto-grants-2008_12