HRID1026238

反应详情

EQUATION

反应方程式

HRID 1026238 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A dichloromethane solution (1.0 M, 150 mL) of tribromoborane was added dropwise to a solution of (2-bromo-4-methoxyphenyl)acetic acid (15.0 g) in dichloromethane (160 mL) at room temperature, and the reaction mixture was refluxed for 3 hr, allowed to cool to room temperature, and poured into ice water. The mixture was extracted with ethyl acetate, and the organic layer was separated. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained yellow solid was collected by filtration and washed with hexane-diethyl ether to give the title compound (10.3 g).

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 3 hr
  2. extractionThe mixture was extracted with ethyl acetate
  3. customthe organic layer was separated
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. filtrationThe obtained yellow solid was collected by filtration
  7. washwashed with hexane-diethyl ether