HRID477435

反应详情

EQUATION

反应方程式

HRID 477435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of benzyl 4-hydroxyphenyl ketone (12.5 g; 0.059 mol), potassium carbonate (11.2 g; 0.08 mol) and sodium iodide (0.5 g) in dimethylformamide (80 ml) was heated to 130° C. At this temperature, 2,2,2-trifluoroethyl p-toluenesulphonate (16.4 g; 0.066 mol), dissolved in dimethyl sulphoxide (30 ml), was added dropwise over 30 minutes. It was then stirred for 45 minutes at a 130° C. After cooling, the reaction mixture was poured into ice-water (500 ml) and the precipitate separated. This was recrystallised from diisopropyl ether/hexane to give pure benzyl 4-(2,2,2-trifluoroethoxy)phenyl ketone.

WORKUP

后处理

  1. additionwas added dropwise over 30 minutes
  2. temperatureAfter cooling
  3. customthe precipitate separated
  4. customThis was recrystallised from diisopropyl ether/hexane