HRID339469

反应详情

EQUATION

反应方程式

HRID 339469 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

To a mixture of 2-(5-bromo-2-ethylphenyl)cyclopentane-1,3-dione (0.200 g, 0.71 mmol), 3,4-dichlorophenol (0.577 g, 3.56 mmol), cesium carbonate (0.502 g, 1.42 mmol), copper triflate (13 mg, 0.04 mmol) and activated (powdered) 5 Å molecular sieves (0.400 g) is added anhydrous toluene (2.5 ml). The reaction mixture is purged with nitrogen then heated at 160° C. for 1 hour under microwave irradiation. After cooling to room temperature dichloromethane is added and mixture is quenched with 2M aqueous hydrochloric acid then filtered. The organic phase is concentrated under reduced pressure to give a crude oil which is purified by preparative reverse-phase HPLC to afford 2-[5-(3,4-dichlorophenoxy)-2-ethylphenyl]cyclopentane-1,3-dione.

WORKUP

后处理

  1. customThe reaction mixture is purged with nitrogen
  2. temperatureAfter cooling to room temperature dichloromethane
  3. additionis added
  4. custommixture is quenched with 2M aqueous hydrochloric acid
  5. filtrationthen filtered
  6. concentrationThe organic phase is concentrated under reduced pressure
  7. customto give a crude oil which
  8. customis purified by preparative reverse-phase HPLC