HRID2393674

反应详情

EQUATION

反应方程式

HRID 2393674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2 equivalents (0.08 mol) of t-butyllithium in pentane are added over the course of one hour at 0° C. to a solution of 8 g (0.04 mol) of bromomesitylene in 100 ml of hexane. The mixture is refluxed for 3 hours. After cooling to 0° C., a solution of 4.17 g (0.01 mol) of 1,4-bis(dibromoboryl)benzene in 80 ml of hexan is added to the mixture and the batch is refluxed overnight. The thick suspension produced is poured into 200 ml of water and subjected twice to extraction with 50 ml of hexane. The combined organic phases are dried over magnesium sulphate, filtered and concentrated. A yellow solid is formed which is recrystallized from hexane, giving 3.0 g (52% of theory) of 1,4-bis(dimesitylboryl)benzene.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 3 hours
  2. temperaturethe batch is refluxed overnight
  3. customThe thick suspension produced
  4. extractionsubjected twice to extraction with 50 ml of hexane
  5. dry with materialThe combined organic phases are dried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customA yellow solid is formed which
  9. customis recrystallized from hexane