HRID1642843

反应详情

EQUATION

反应方程式

HRID 1642843 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

At −78° C., 8.5 ml (1.4 g, 21.1 mmol) of a 2.5M solution of n-butyllithium in hexane were initially charged in 30 ml of THF. 4.9 g (19.2 mmol) of 4-bromo-2-methyl(trifluoromethoxy)benzene were dissolved in 15 ml of THF and slowly added dropwise. 3.0 g (28.8 mmol) of trimethylboronic acid were then added dropwise. The mixture was stirred at −78° C. for 2 h, and 11 ml of 2 N hydrochloric acid were then added. The mixture was allowed to warm to RT, and the organic phase was separated off. The solvent was removed under reduced pressure and the residue was recrystallized from n-heptane. Yield: 3.3 g (78% of theory)

WORKUP

后处理

  1. additionslowly added dropwise
  2. temperatureto warm to RT
  3. customthe organic phase was separated off
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was recrystallized from n-heptane