HRID1062923

反应详情

EQUATION

反应方程式

HRID 1062923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Using a method similar to Example 15 a), 6.75 g (0.03 mol) of (2), 8.5 g (0.033 mol) of 3,5-bis(trifluoromethyl)phenylboronic acid and 7.0 g (0.066 mol) of sodium carbonate were placed in 120 ml of dimethoxyethane and 36 ml of water in the reaction vessel, the mixture was degassed a number of times and saturated with argon. 120 mg (0.5 mmol) of palladium acetate and 282 mg (1.1 mmol) of TPP were added and the reaction mixture was stirred for 2 hours at 80° C. After addition of 150 ml of water, the mixture was extracted 3 times with 150 ml each time of diethyl ether, the combined ether phases were washed 3 times with 150 ml each time of water and dried over magnesium sulfate. Removal of the solvent gave 9.93 g of (18) as an oil.

WORKUP

后处理

  1. custom36 ml of water in the reaction vessel, the mixture was degassed a number of times
  2. extractionthe mixture was extracted 3 times with 150 ml each time of diethyl ether
  3. washthe combined ether phases were washed 3 times with 150 ml each time of water
  4. dry with materialdried over magnesium sulfate
  5. customRemoval of the solvent