HRID18697

反应详情

EQUATION

反应方程式

HRID 18697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 18 (2 g, 4.84 mmol), AIBN (0.08 g, 0.48 mmol), Bu3SnH (3.91 ml, 14.50 mmol) in toluene (49 ml) was heated to reflux for 15 h. After cooling, the reaction mixture was evaporated and then extracted by CH2Cl2. The combined organic layer was dried by MgSO4 and concentrated to give a residue that was purified by silica gel flash column chromatography (EtOAc:n-hexane=1:2) to give compound 19, yield 90%.

WORKUP

后处理

  1. temperatureto reflux for 15 h
  2. temperatureAfter cooling
  3. customthe reaction mixture was evaporated
  4. extractionextracted by CH2Cl2
  5. dry with materialThe combined organic layer was dried by MgSO4
  6. concentrationconcentrated
  7. customto give a residue that
  8. customwas purified by silica gel flash column chromatography (EtOAc:n-hexane=1:2)