HRID1694733

反应详情

EQUATION

反应方程式

HRID 1694733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The product from example 32 step (ii) (0.5 g) and 4-bromo-3-chloroaniline (0.38 g) were dissolved in toluene (4 ml). Ethanol (1 ml), 2M aqueous sodium carbonate (1 ml) and Pd(PPh3)4 (0.115 g) were added sequentially and the mixture heated at reflux for 4 h. The reaction was cooled, evaporated, dissolved in EtOAc, washed with water and brine, dried (MgSO4) and evaporated. The residue was purified by chromatography on silica eluting with 10% EtOAc/isohexane. Yield 0.23 g.

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 4 h
  3. temperatureThe reaction was cooled
  4. customevaporated
  5. dissolutiondissolved in EtOAc
  6. washwashed with water and brine
  7. dry with materialdried (MgSO4)
  8. customevaporated
  9. customThe residue was purified by chromatography on silica eluting with 10% EtOAc/isohexane