HRID1824308

反应详情

EQUATION

反应方程式

HRID 1824308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium carbonate (24 g) was added to a solution of of 2-methoxy phenol (18.94 g, 0.152 mol) in acetone (500 ml) at room temperature. A solution of bromoacetonitrile (17.43 g, 0.145 mol) in acetone (500 ml) was then added and the resulting suspension was heated at reflux for 10 h. The reaction vessel was then cooled and the solution was concentrated under reduced pressure and taken up into water (150 ml). Chloroform (250 ml) was added and the two layers separated. The organic phase was washed with brine (100 ml) and 10% aqueous NaOH (100 ml). The organic phase was dried (MgSO4) and concentrated under reduced pressure to give the product (19.91 g, 80%) as an oil. 1H NMR (CDCl3, 250 MHz) 7.0 (4H m), 4.8 (2H, s), 3.9 (3H, s).

WORKUP

后处理

  1. temperaturethe resulting suspension was heated
  2. temperatureat reflux for 10 h
  3. temperatureThe reaction vessel was then cooled
  4. concentrationthe solution was concentrated under reduced pressure
  5. additionChloroform (250 ml) was added
  6. customthe two layers separated
  7. washThe organic phase was washed with brine (100 ml) and 10% aqueous NaOH (100 ml)
  8. dry with materialThe organic phase was dried (MgSO4)
  9. concentrationconcentrated under reduced pressure