HRID1082284

反应详情

EQUATION

反应方程式

HRID 1082284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butyl 4-{2-{6-(4-tert-butylbenzenesulfonylamino)-5-(4-methylphenyl)pyrimidin-4-yloxy]ethoxy}phenoxyacetate (1.25 g) in dichloromethane (120 ml) are added anisole (2.09 g) and trifluoroacetic acid (20 ml) under ice-cooling. The mixture is stirred at room temperature for five hours, washed with water, and extracted with 10% aqueous sodium hydroxide solution. The aqueous layer is washed with chloroform, and acidified with 10% hydrochloric acid under ice-cooling. The mixture is extracted with ethyl acetate, and the extract is washed, dried, and evaporated to remove the solvent. The residue is crystallized from ethyl acetate/diisopropyl ether to give 4-{2-[6-(4-tert-butylbenzenesulfonylamino )-5-(4-methylphenyl)pyrimidin-4-yloxy]ethoxy}phenoxyacetic acid (1.14 g).

WORKUP

后处理

  1. temperaturecooling
  2. washwashed with water
  3. extractionextracted with 10% aqueous sodium hydroxide solution
  4. washThe aqueous layer is washed with chloroform
  5. temperaturecooling
  6. extractionThe mixture is extracted with ethyl acetate
  7. washthe extract is washed
  8. customdried
  9. customevaporated
  10. customto remove the solvent
  11. customThe residue is crystallized from ethyl acetate/diisopropyl ether