HRID321919

反应详情

EQUATION

反应方程式

HRID 321919 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

4.12 ml (10.3 mmoles) of n-BuLi 2.5 M in hexane are added to a solution of 1.48 g of 4,7-dimethyl indene (XVIII) (10.3 mmoles; obtained as described above) in 55 ml of a mixture of THF-hexane 2/1. At the end of the addition, the mixture is left under stirring for 1 hour. It is then cooled to −70° C. and a solution of 2.3 g of the brominated compound having formula (XX) (7.37 mmoles) in THF/hexane are added dropwise. The mixture is left to rise to room temperature and is left to rest for 6 hours. It is then poured into water and is extracted with ethyl ether. The organic phase is washed until neutrality and dehydrated on sodium sulfate. The residue obtained by evaporation of the solvent is purified by silica gel chromatography eluating with petroleum ether. After evaporation of the eluant 2.0 g of the bis-indenyl ligand having formula (XXI) and indicated below, are obtained (72% yield).

WORKUP

后处理

  1. additionAt the end of the addition
  2. waitthe mixture is left
  3. additionare added dropwise
  4. waitThe mixture is left
  5. customto rise to room temperature
  6. waitis left
  7. waitto rest for 6 hours
  8. extractionis extracted with ethyl ether
  9. washThe organic phase is washed until neutrality
  10. customThe residue obtained by evaporation of the solvent
  11. customis purified by silica gel chromatography
  12. customAfter evaporation of the eluant 2.0 g of the bis-indenyl ligand
  13. customare obtained (72% yield)