HRID503918

反应详情

EQUATION

反应方程式

HRID 503918 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of NaOH (5.72 g, 143 mmol) in water (29 mL) was added to a solution of (4-bromo-2-methoxy-phenyl)-acetonitrile (10.2 g, 45.1 mmol) in MeOH (100 mL). The reaction mixture was heated at reflux for 18 hours. The solvent was evaporated under reduced pressure and water was added. The aqueous mixture was washed with diethyl ether, and the aqueous layer was acidified by addition of aqueous HCl (2 M) to pH 1. The aqueous mixture was then extracted with EtOAc, and the combined organic extracts were washed with brine, dried over Na2SO4, filtered, and evaporated under reduced pressure to give 9.49 g (86% yield) of (4-bromo-2-methoxy-phenyl)-acetic acid.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 18 hours
  3. customThe solvent was evaporated under reduced pressure and water
  4. additionwas added
  5. washThe aqueous mixture was washed with diethyl ether
  6. additionthe aqueous layer was acidified by addition of aqueous HCl (2 M) to pH 1
  7. extractionThe aqueous mixture was then extracted with EtOAc
  8. washthe combined organic extracts were washed with brine
  9. dry with materialdried over Na2SO4
  10. filtrationfiltered
  11. customevaporated under reduced pressure