반응 #945025

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biscyclopentadienyidimethylsilane

2-bromo-1-trimethylsiloxyethane

→

(2-trimethylsiloxyethylcyclopentadienyl) dimethyl cyclopentadienyl silane

수율 52.0%

용매

THF

THF

THF

THF

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후처리

1. 1
   기타A purple solution was immediately formed
2. 2
   기타Then, the volatiles were removed
3. 3
   세척the residue was washed with hexane
4. 4
   기타to give a pink solid
5. 5
   기타A pink suspension was immediately formed
6. 6
   기타the solvents were removed
7. 7
   workup.ADDITIONthe residue was treated with hexane
8. 8
   여과the supernatant solution was filtered
9. 9
   기타The removal of the hexane
10. 10
    workup.DISTILLATIONThis oil was distilled in order
11. 11
    기타to obtain a yellow oil, which

실험 절차

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).

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