HRID1291302

反应详情

EQUATION

反应方程式

HRID 1291302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of theophylline (1.80 g) in DMF (20 ml) were added potassium carbonate (1.66 g) and 4-[4-(trifluoromethyl)benzoyl]benzyl bromide (3.43 g) and the mixture was stirred at room temperature for 20 hours. This reaction mixture was diluted with water and extracted with ethyl acetate. The extract was washed with saturated aqueous NaCl solution and dried over anhydrous sodium sulfate and the solvent was distilled off. To the residue was added 4N-hydrogen chloride/ethyl acetate and the resulting precipitate was harvested by filtration. To this precipitate was added a saturated aqueous solution of NaHCO3 and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous NaCl solution and dried over anhydrous sodium sulfate and the solvent was distilled off to provide the title compound as colorless powder (1.57 g, 36%).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated aqueous NaCl solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off
  5. additionTo the residue was added 4N-hydrogen chloride/ethyl acetate
  6. filtrationthe resulting precipitate was harvested by filtration
  7. additionTo this precipitate was added a saturated aqueous solution of NaHCO3
  8. extractionthe mixture was extracted with ethyl acetate
  9. washThe extract was washed with saturated aqueous NaCl solution
  10. dry with materialdried over anhydrous sodium sulfate
  11. distillationthe solvent was distilled off