反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionAt the end of the addition
- waitthe mixture is left
- additionare added dropwise
- waitThe mixture is left
- customto rise to room temperature
- waitis left
- waitto rest for 6 hours
- extractionis extracted with ethyl ether
- washThe organic phase is washed until neutrality
- customThe residue obtained by evaporation of the solvent
- customis purified by silica gel chromatography
- customAfter evaporation of the eluant 2.0 g of the bis-indenyl ligand
- customare obtained (72% yield)