HRID991429

反应详情

EQUATION

反应方程式

HRID 991429 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3,4-dimethoxybenzoyl chloride (0.5 g), N-(5-amino-4-chloro-2-fluorophenyl)-3-dimethylaminobenzamide (0.781 g) and pyridine (8 ml) was stirred at ambient temperature for 18 hours. The mixture was evaporated and the residue was partitioned between methylene chloride and a saturated aqueous copper sulphate solution. The organic phase was washed in turn with water and a saturated aqueous sodium chloride solution, dried (MgSO4) and evaporated. The residue was purified by column chromatography on silica using a 99:1 mixture of methylene chloride and methanol as eluent. There was thus obtained the title compound as a solid (0.328 g);

WORKUP

后处理

  1. customThe mixture was evaporated
  2. customthe residue was partitioned between methylene chloride
  3. washThe organic phase was washed in turn with water
  4. dry with materiala saturated aqueous sodium chloride solution, dried (MgSO4)
  5. customevaporated
  6. customThe residue was purified by column chromatography on silica using
  7. additiona 99:1 mixture of methylene chloride and methanol as eluent