HRID733046

反应详情

EQUATION

反应方程式

HRID 733046 的结构方程式

PROCEDURE

实验过程

4-Bromo-2-phenoxy-benzonitrile (35.3 g, 129 mmol) was added to 130 mL EtOH, followed by the addition of 340 mL of 20% NaOH (aq). The reaction was heated to reflux for 20 h. The mixture was cooled to room temperature and poured into 6 N HCl to form a precipitate. The solid was collected by vacuum filtration and dissolved in 3:1 THF-ethyl ether and washed with brine. The organic phase was dried over magnesium sulfate, and concentrated. The solids were dried in a vacuum oven at 60° C. overnight to give 35.1 g (128 mmol) of the desired product. MS m/z (MH+) 292.

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 20 h
  3. customto form a precipitate
  4. filtrationThe solid was collected by vacuum filtration
  5. dissolutiondissolved in 3:1 THF-ethyl ether
  6. washwashed with brine
  7. dry with materialThe organic phase was dried over magnesium sulfate
  8. concentrationconcentrated
  9. customThe solids were dried in a vacuum oven at 60° C. overnight