HRID465528

反应详情

EQUATION

反应方程式

HRID 465528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a solution of 0.879 g (7 mmol) of 4-ethenyltetrahydro-2H-pyran-2-one in 5 ml triethylamine and 5 ml acetonitrile is added 0.081 g (0.36 mmol) Palladium-(II)-acetate followed by 0.659 g (2.5 mmol) tri-o-tolylphosphine and 0.76 ml (7.9 mmol) 3-bromopyridine and the mixture is heated at 125° for 20 h in a sealed tube. It is then cooled, diluted with methylene chloride and washed with water. The organic phase is dried (MgSO4), filtered and evaporated to give a reddish oil which is flash chromatographed using ethyl acetate as eluent to obtain 4-[2-(3-pyridyl)ethenyl]-tetrahydro-2H-pyran-2-one as an oil.

WORKUP

后处理

  1. temperaturethe mixture is heated at 125° for 20 h in a sealed tube
  2. temperatureIt is then cooled
  3. washwashed with water
  4. dry with materialThe organic phase is dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customto give a reddish oil which
  8. customchromatographed