反应详情

A 300 ml two-necked flask equipped with a three-way cock, a dropping funnel and a magnetic stirrer, was thoroughly purged with nitrogen. The above-obtained chlorodicyclohexyl(2,7-di-tert-butylfluorenyl)silane 5.5 g (11.0 mmol) and dehydrated diethyl ether 30 ml were placed in the flask. Hexamethylphosphoric triamide 3.0 ml was further added. With the flask cooled in an ice bath, 2.0 mol/L tetrahydrofuran solution of cyclopentadienyl sodium, 11.0 ml (22.0 mmol), was gradually added. After the liquid temperature was slowly raised to room temperature, the contents were stirred for 2 days in a nitrogen atmosphere at room temperature to give a slurry. To the slurry, 1 N hydrochloric aqueous solution acid 100 ml was added, and the water phase was removed by means of a 300 ml separatory funnel. The organic phase thus obtained was washed twice with water 100 ml and once with a saturated salt solution 100 ml, and dried over anhydrous magnesium sulfate. The solution was filtered to remove the magnesium sulfate, and the solvent of the filtrate was distilled away to obtain a solid. The solid was washed with n-hexane and then dried to give 1.514 g of dicyclohexylcyclopentadienyl(2,7-di-tert-butylfluorenyl)silane as a white solid (2.82 mmol, 26% yield). The 1H NMR spectrum and the FD-MS spectrum as measured with respect to the dicyclohexylcyclopentadienyl(2,7-di-tert-butylfluorenyl)silane are given below:

1. customA 300 ml two-necked flask equipped with a three-way cock, a dropping funnel and a magnetic stirrer
2. customwas thoroughly purged with nitrogen
3. temperatureWith the flask cooled in an ice bath
4. customto give a slurry
5. customthe water phase was removed by means of a 300 ml separatory funnel
6. customThe organic phase thus obtained
7. washwas washed twice with water 100 ml and once with a saturated salt solution 100 ml
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationThe solution was filtered
10. customto remove the magnesium sulfate
11. distillationthe solvent of the filtrate was distilled away
12. customto obtain a solid
13. washThe solid was washed with n-hexane
14. customdried