HRID1267110

反应详情

EQUATION

反应方程式

HRID 1267110 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 5′-chloro-2′-methyl-4-trifluoromethyl-biphenyl (27 g) in a mixture of t-butanol (100 mL) and H2O (200 mL) was added portionwise KMnO4 (46.9 g). At the end of the addition, the mixture was heated under reflux for 16 hours, cooled to room temperature and filtered on celite. The filtrate was then acidified with concentrated HCl and the aqueous layer was extracted with AcOEt. The combined organic extracts were washed with brine, dried over Na2SO4, filtered and evaporated under reduced pressure to give the title compound (24 g) as white crystals.

WORKUP

后处理

  1. additionAt the end of the addition
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 16 hours
  4. filtrationfiltered on celite
  5. extractionthe aqueous layer was extracted with AcOEt
  6. washThe combined organic extracts were washed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. customevaporated under reduced pressure