HRID521544

反应详情

EQUATION

反应方程式

HRID 521544 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

A mixture of 6 (4.11 g, 10.3 mmol), 7 (4.60 g, 10.3 mmol), tetrakis(triphenylphosphine)palladium(0) (0.595 g, 0.515 mmol), Na2CO3 (5.41 g, 51.0 mmol), H2O (55 mL) and THF (92 mL) was degassed with argon for about 1 h while stirring. The stirring reaction mixture was then maintained under argon at about 80° C. for about 18 h. Upon confirming consumption of the starting materials by TLC (SiO2, 49:1 dichloromethane-acetone), the reaction was cooled to RT, filtered and filtrant washed with EtOAc and H2O to afford 8 (5.92 g, 90%) as an off-white solid.

WORKUP

后处理

  1. customwas degassed with argon for about 1 h
  2. customThe stirring reaction mixture
  3. customconsumption of the starting materials by TLC (SiO2, 49:1 dichloromethane-acetone)
  4. temperaturethe reaction was cooled to RT
  5. filtrationfiltered
  6. washfiltrant washed with EtOAc and H2O