HRID1771773

反应详情

EQUATION

反应方程式

HRID 1771773 的结构方程式

PROCEDURE

实验过程

A solution of 2-[3-[[2-fluoro-5-(3-fluorophenyl)phenyl]methylamino]-2,4-dimethyl-phenoxy]acetic acid (I(j)) (120 mg, 0.3 mmol, 1 eq) and SOCl2 (1 mL) in i-PrOH (4 mL) was heated at reflux for 2 h. The solvent was evaporated in vacuo and the residue was taken up in water and basified to pH 8 by addition of aqueous NaHCO3. The mixture was extracted with EtOAc and the organic extract was dried (Na2SO4) filtered and evaporated in vacuo. The residue obtained was purified by column chromatography to give the title compound as an oil (120 mg, 90%).

WORKUP

后处理

  1. temperatureat reflux for 2 h
  2. customThe solvent was evaporated in vacuo
  3. additionthe residue was taken up in water and basified to pH 8 by addition of aqueous NaHCO3
  4. extractionThe mixture was extracted with EtOAc
  5. extractionthe organic extract
  6. dry with materialwas dried (Na2SO4)
  7. filtrationfiltered
  8. customevaporated in vacuo
  9. customThe residue obtained
  10. customwas purified by column chromatography