HRID1363871

反应详情

EQUATION

反应方程式

HRID 1363871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,5-Bis(trifluoromethyl) phenol (20.6 g) was dissolved in 1N sodium hydroxide (270 mL). The solution was refluxed under heating for 10 hours. After addition of 11-bromododecanoic acid (4.7 g), the solution was kept refluxed under heating, and then left to be cooled. The reaction solution was added with 1N aqueous hydrochloric acid and extracted with ethyl acetate. The resulting organic layer was dried over anhydrous magnesium sulfate, and the solvent was removed. The resulting crystals was washed with hexane and purified by silica gel column chromatography to obtain 11-(3,5-bis(trifluoromethyl) phenoxy)dodecanoic acid (18.4 g, 50%).

WORKUP

后处理

  1. temperatureThe solution was refluxed
  2. temperatureunder heating for 10 hours
  3. temperaturethe solution was kept refluxed
  4. temperatureunder heating
  5. waitleft
  6. temperatureto be cooled
  7. extractionextracted with ethyl acetate
  8. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  9. customthe solvent was removed
  10. washThe resulting crystals was washed with hexane
  11. custompurified by silica gel column chromatography