反应详情

A solution of 11.5 g (61 mmol) of biscyclopentadienyidimethylsilane in THF was added to a suspension of 1.3 g (55 mmol) of HK in THF at −78° C. A purple solution was immediately formed. Then, the volatiles were removed and the residue was washed with hexane to give a pink solid. The solid was solved again in THF and a solution of 10.8 g (55 mmol) of 2-bromo-1-trimethylsiloxyethane in THF was added at room temperature. A pink suspension was immediately formed. The mixture was stirred for 12 h, and then the solvents were removed, the residue was treated with hexane and the supernatant solution was filtered. The removal of the hexane led to a reddish oil. This oil was distilled in order to obtain a yellow oil, which was characterized as a mixture of position isomers of (2-trimethylsiloxyethylcyclopentadienyl) dimethyl cyclopentadienyl silane (Tb: 135–140° C.; 1 mm Hg), (8.7 g, 28.6 mmol, yield: 52%). 1H-RMN(CDCl3): 6.82–6.40 (m, 7H); 3.82 (m, 2H); 3.10 (m, 2H); 2.73 (m, 2H); 0.20 (s, 15 H).

1. customA purple solution was immediately formed
2. customThen, the volatiles were removed
3. washthe residue was washed with hexane
4. customto give a pink solid
5. customA pink suspension was immediately formed
6. customthe solvents were removed
7. additionthe residue was treated with hexane
8. filtrationthe supernatant solution was filtered
9. customThe removal of the hexane
10. distillationThis oil was distilled in order
11. customto obtain a yellow oil, which