HRID459541

反应详情

EQUATION

反应方程式

HRID 459541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

4-Bromopyridine hydrochloride (11.7 g) and 4-carboxyphenylboric acid (10.0 g) were dissolved in a mixed solvent of toluene (250 ml) and water (250 ml), tetrakis(triphenylphosphine)palladium(0) (5.0 g) and anhydrous sodium carbonate (25.4 g) were successively added, and the mixture was heated under reflux at 120° C. for 19 hours. After the reaction mixture was cooled to room temperature, ethyl acetate was added to the reaction mixture to extract it with water. Concentrated hydrochloric acid was added to the water layer to acidify it. The water layer was washed with ethyl acetate and then concentrated, and solids deposited were collected to obtain the title compound (8.37 g) as a colorless solid.

WORKUP

后处理

  1. additionwere successively added
  2. temperaturethe mixture was heated
  3. temperatureAfter the reaction mixture was cooled to room temperature
  4. extractionto extract it with water
  5. additionConcentrated hydrochloric acid was added to the water layer
  6. washThe water layer was washed with ethyl acetate
  7. concentrationconcentrated
  8. customsolids deposited were collected