HRID1533117

反应详情

EQUATION

反应方程式

HRID 1533117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

25 g (0.1322 mol) of 2′,4′-dichloroacetophenone was placed in a three-neck round bottom flask equipped with a magnetic stir bar, reflux condenser, and dropping funnel. Anhydrous ether (30 mL) and AlCl3 (0.20 g) were added. The solution was stoppered and cooled to 0° C. in an ice bath. Br2 (21.13 g, 0.1322 mol) was added dropwise (at a rate of approximately 0.5 mL/min). After addition of Br2 was complete, HBr and the solvent were removed under reduced pressure. The remaining HBr was removed by blowing a stream of nitrogen over the orange oily product. The resulting oil was placed under high vacuum until all the bubbling had ceased. The product was obtained as a viscous orange oil, which solidified upon standing in the refrigerator. Yield: 35.72 g (100%); TLC: 95% Hexanes/5% Acetone, Rf=0.35.

WORKUP

后处理

  1. customequipped with a magnetic stir bar
  2. temperaturereflux condenser
  3. customHBr and the solvent were removed under reduced pressure
  4. customThe remaining HBr was removed
  5. customThe product was obtained as a viscous orange oil, which