HRID1172762

反应详情

EQUATION

反应方程式

HRID 1172762 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

In an argon atmosphere, 50 mL of dehydrated THF were added to 3.5 g (8.6 mmol) of 2-bromo-9,10-diphenylanthracene, and the temperature of the mixture was cooled to −78° C. Then, 6.0 mL of n-butyllithium (in hexane, 1.6 mol/L) were dropped. After the mixture had been stirred at −78° C. for 1 hour, the temperature of the mixture was increased to 0° C. The temperature of the mixture was cooled to −78° C. again, and 2.9 mL (26 mmol) of trimethoxyborane were dropped. The mixture was stirred at −78° C. for 1 hour, and was then stirred at room temperature for 2 hours. 50 mL of 10-mass % hydrochloric acid were added, and the whole was stirred for 1 hour, followed by filtration. The resultant solid was washed with toluene to obtain 2.6 g of 9,10-diphenylanthracene-2-boronic acid (80% yield).

WORKUP

后处理

  1. temperaturethe temperature of the mixture was increased to 0° C
  2. temperatureThe temperature of the mixture was cooled to −78° C. again
  3. stirringThe mixture was stirred at −78° C. for 1 hour
  4. stirringwas then stirred at room temperature for 2 hours
  5. stirringthe whole was stirred for 1 hour
  6. filtrationfollowed by filtration
  7. washThe resultant solid was washed with toluene