HRID2268112

反应详情

EQUATION

反应方程式

HRID 2268112 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

A solution of 13 g of 2-bromo-4,6-di-tert.butyl-phenol in 100 ml of dimethylformamide (DMF) was added dropwise to a suspension of 2.2 g of sodium hydride (50% in mineral oil) in 100 ml of DMF at 0° C. The reaction mixture was stirred at room temperature until hydrogen was no longer evolved (ca. 1 h), cooled again to 0° C. and treated with a solution of 22 g of ethyl iodide in 50 ml of DMF. After stirring for about 1 hour at room temperature, the reaction mixture was poured on icewater, extracted with ethyl acetate, washed (H2O), dried (Na2SO4) and evaporated to give 13.5 g of 1-bromo-2-ethoxy-3,5-di-tert.butyl-benzene as white crystals, m.p. 55-56° C.

WORKUP

后处理

  1. custom(ca. 1 h)
  2. additionthe reaction mixture was poured on icewater
  3. extractionextracted with ethyl acetate
  4. washwashed (H2O)
  5. dry with materialdried (Na2SO4)
  6. customevaporated