HRID1860586

反应详情

EQUATION

反应方程式

HRID 1860586 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To stirred solution of 1-(3-methyl-4-methoxyphenyl)ethanone (3.29 g, 20 mmol) in DME was added ethyl trifluoroacetate (5.68 g, 40 mmol) and sodium methoxide (4.32 g, 80 mmol), and the resulting reaction mixture was stirred at room temperature overnight. EtOAc (200 ml) and water (50 ml) were added, and the pH of the aqueous layer was adjusted to 6 by addition of 1 N HCl solution. The organic layer was washed with brine (50 ml), dried over Na2SO4, and concentrated in vacuo to give the crude product which was recrystallized from isooctane to give the title compound (3.2 g, 62%).

WORKUP

后处理

  1. customthe resulting reaction mixture
  2. washThe organic layer was washed with brine (50 ml)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customto give the crude product which
  6. customwas recrystallized from isooctane