HRID1916578

反应详情

EQUATION

反应方程式

HRID 1916578 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

210 mg (0.86 mmol) Pd(OAc)2, 5.23 g (17.32 mmol) tetra-n-butylammonium chloride and 3.6 g NaHCO3 are added to a solution of 5.0 g (17.32 mmol) 4-bromo-iodo-benzene and 3.0 mL (43.67 mmol) allylalcohol in 30 mL DMF. The reaction solution is stirred for 2 h at 60° C. and diluted with 50 mL water. The aqueous phase is extracted with 50 mL EtOAc and the combined organic extracts are washed with 50 mL saturated NaCl solution. The organic phase is dried over Na2SO4 and the solvent is eliminated i.vac. Further purification is carried out by column chromatography on silica gel (cyc/EtOAc 3:1).

WORKUP

后处理

  1. extractionThe aqueous phase is extracted with 50 mL EtOAc
  2. washthe combined organic extracts are washed with 50 mL saturated NaCl solution
  3. dry with materialThe organic phase is dried over Na2SO4
  4. customFurther purification