HRID2298465

反应详情

EQUATION

反应方程式

HRID 2298465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

22.5 g (0.1 mol) of 7-bromo-2-methyl-1-indanone (2), 13.4 g (0.11 mol) of phenylboronic acid and 23.3 g (0.22 mol) of sodium carbonate were placed in 380 ml of dimethoxyethane and 120 ml of water in the reaction vessel, the mixture was degassed a number of times and saturated with argon. 450 mg (2 mmol) of palladium acetate and 1.05 g (4 mmol) of triphenylphosphine (TPP) were added and the reaction mixture was stirred for 2 hours at 80° C. After addition of 300 ml of water, the mixture was extracted 3 times with 250 ml each time of diethyl ether, the ether phase was washed twice with 100 ml each time of water and dried over magnesium sulfate. Removal of the solvent gave 21.1 g of (15) as solid.

WORKUP

后处理

  1. custom120 ml of water in the reaction vessel, the mixture was degassed a number of times
  2. extractionthe mixture was extracted 3 times with 250 ml each time of diethyl ether
  3. washthe ether phase was washed twice with 100 ml each time of water
  4. dry with materialdried over magnesium sulfate
  5. customRemoval of the solvent