HRID452242

反应详情

EQUATION

反应方程式

HRID 452242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2.00 g (6.19 mmol) of the compound from Example 51A are dissolved in 31 ml of anhydrous dioxane, and 2.36 g (7.42 mmol) of tributylvinyltin and 143 mg (0.124 mmol) of tetrakis(triphenylphosphine)palladium are added and the mixture is stirred at 100° C. for 5 h. The mixture is allowed to cool and filtered through kieselguhr. The filter cake is washed three times with ethyl acetate, and the combined filtrates are concentrated to dryness under reduced pressure. The residue is purified by chromatography on silica gel (cyclohexane/ethyl acetate 4:1). This gives 846 mg (51% of theory) of the desired product.

WORKUP

后处理

  1. temperatureto cool
  2. filtrationfiltered through kieselguhr
  3. washThe filter cake is washed three times with ethyl acetate
  4. concentrationthe combined filtrates are concentrated to dryness under reduced pressure
  5. customThe residue is purified by chromatography on silica gel (cyclohexane/ethyl acetate 4:1)