HRID648875

反应详情

EQUATION

反应方程式

HRID 648875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

4'-(2-Methylbutyloxy)-4-hydroxybiphenyl (15 g) obtained in Example 1, (i) was dissolved in 1,4-dioxane (50 ml), followed by dropwise adding a mixture of bromine (10.5 g) and 1,4-dioxane (140 ml), heating on a water bath at 40° C. for 4 hours with stirring, thereafter distilling off 1,4-dioxane under reduced pressure, adding toluene (300 ml) to the remaining solution, adding a 10% aqueous solution of sodium hydrogen sulfite till the color of bromine disappeared, three times washing with saturated aqueous solution of NaCl to make the liquid neutral, drying and distilling off toluene to obtain a raw product of 4'-(2-methylbutyloxy-3-bromo-4-hydroxybiphenyl (21 g).

WORKUP

后处理

  1. additionby dropwise adding
  2. distillationdistilling off 1,4-dioxane under reduced pressure
  3. additionadding toluene (300 ml) to the remaining solution
  4. additionadding a 10% aqueous solution of sodium hydrogen sulfite till the color of bromine
  5. washthree times washing with saturated aqueous solution of NaCl
  6. customdrying
  7. distillationdistilling off toluene