反应 #5070

ord-2bbab0f4ae63457f992a8d6c141b0c62

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The solution was heated
  2. 2
    温度at reflux
  3. 3
    workup.STIRRINGto stir under N2 for 15 minutes
  4. 4
    洗涤washed with water
  5. 5
    萃取The organic extract
  6. 6
    干燥was dried (MgSO4)
  7. 7
    其他evaporated in vacuo

实验过程

Methyl 3-iodobenzoate (13 g) and vinyl tributyltin (20 g) were dissolved in toluene (100 ml) and tetrakis(triphenylphosphine)palladium (0) (500 mg) added. The solution was heated at reflux with stirring under N2 for 1 day. Potassium fluoride (3 g) in water (50 ml) was added and the reaction mixture was allowed to stir under N2 for 15 minutes. The product was taken up in ethyl acetate and washed with water and then brine (×2). The organic extract was dried (MgSO4) and evaporated in vacuo.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05242930uspto-grants-1993_09