HRID1766080

反应详情

EQUATION

反应方程式

HRID 1766080 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Chloro-5-cyano-4-(3-methoxyphenyl)-2-methylthio-pyrimidine (example 1b, 1.46 g) was suspended in 1,4-dioxane (10 ml). Tetrakis(triphenylphosphine)palladium(0) (350 mg) was added and the mixture was flushed with a nitrogen atmosphere. Tetravinyltin (1.26 ml) was added and the mixture was refluxed for 5 h. The reaction mixture was then poured in a mixture of EtOAc (100 ml) and H2O (100 ml). The organic layer was washed with sat. aq. NaCl, dried (MgSO4) and concentrated under reduced pressure. The title compound was purified by chromatography on silica gel with hept/CH2Cl2=1/0 to 1/3 (v/v).

WORKUP

后处理

  1. customthe mixture was flushed with a nitrogen atmosphere
  2. additionTetravinyltin (1.26 ml) was added
  3. temperaturethe mixture was refluxed for 5 h
  4. additionThe reaction mixture was then poured in a mixture of EtOAc (100 ml) and H2O (100 ml)
  5. washThe organic layer was washed with sat. aq. NaCl
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated under reduced pressure
  8. customThe title compound was purified by chromatography on silica gel with hept/CH2Cl2=1/0 to 1/3 (v/v)