HRID1362519

反应详情

EQUATION

反应方程式

HRID 1362519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3′-Chloro-2′-hydroxypropiophenone (10 g, 54.3 mmol) and potassium carbonate (17.5 g) in 70 ml of acetone are admixed with 7 ml of dimethyl sulphate. The reaction mixture is boiled at reflux for three hours. After it has cooled to room temperature, the batch is subjected to suction filtration through Celite and the filter cake is washed with diethyl ether. After the solvent has been removed on a rotary evaporator, the yellow oil which remains is diluted with 200 ml of diethyl ether and the organic phase is washed with 0.2 M aqueous sodium hydroxide solution (100 ml) and brine (100 ml). The organic phase is dried over sodium sulphate and the solvent is removed on a rotary evaporator. This leaves the desired title compound as a colourless oil (98% yield).

WORKUP

后处理

  1. temperatureat reflux for three hours
  2. filtrationthe batch is subjected to suction filtration through Celite
  3. washthe filter cake is washed with diethyl ether
  4. customAfter the solvent has been removed on a rotary evaporator
  5. additionthe yellow oil which remains is diluted with 200 ml of diethyl ether
  6. washthe organic phase is washed with 0.2 M aqueous sodium hydroxide solution (100 ml) and brine (100 ml)
  7. dry with materialThe organic phase is dried over sodium sulphate
  8. customthe solvent is removed on a rotary evaporator