HRID324466

反应详情

EQUATION

反应方程式

HRID 324466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product from step (ix) (2.8 g) and N-bromosuccinamide were dissolved in ethyl acetate (30 ml) and irradiated with a 500 Watt halogen lamp at reflux for 2 h. The solvent was evaporated under reduced pressure and the solid residue dissolved in dichloromethane (30 ml) and treated with triethylamine (10 ml). After 2 h the solvents were removed under reduced pressure and the residue partioned between water and ethyl acetate. The organic layer was collected and dried over MgSO4. The solvent was evaporated under reduced pressure and the product purified by flash chromatography.

WORKUP

后处理

  1. temperatureat reflux for 2 h
  2. customThe solvent was evaporated under reduced pressure
  3. dissolutionthe solid residue dissolved in dichloromethane (30 ml)
  4. additiontreated with triethylamine (10 ml)
  5. customAfter 2 h the solvents were removed under reduced pressure
  6. customThe organic layer was collected
  7. dry with materialdried over MgSO4
  8. customThe solvent was evaporated under reduced pressure
  9. customthe product purified by flash chromatography