HRID274888

反应详情

EQUATION

反应方程式

HRID 274888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The whole of the solid obtained in Step C is dissolved in 70 ml of toluene and then treated with 1.25 ml (13.3 mmol) of phosphorus oxychloride. The mixture is refluxed for one hour. After returning to room temperature, the reaction mixture is poured onto 60 ml of ice-water and then mixed with 100 ml of diethyl ether. Customary treatment of the organic phase yields, after purification over a silica column (eluant: methylene chloride), 12.36 g of a yellow solid recrystallised from diisopropyl ether.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for one hour
  2. customAfter returning to room temperature
  3. customCustomary treatment of the organic phase yields
  4. customafter purification over a silica column (eluant: methylene chloride), 12.36 g of a yellow solid
  5. customrecrystallised from diisopropyl ether