Reacción #945025

ord-1243a0778270483a8db9ea9a1e0b301c

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroA purple solution was immediately formed
  2. 2
    OtroThen, the volatiles were removed
  3. 3
    Lavadothe residue was washed with hexane
  4. 4
    Otroto give a pink solid
  5. 5
    OtroA pink suspension was immediately formed
  6. 6
    Otrothe solvents were removed
  7. 7
    workup.ADDITIONthe residue was treated with hexane
  8. 8
    Filtraciónthe supernatant solution was filtered
  9. 9
    OtroThe removal of the hexane
  10. 10
    workup.DISTILLATIONThis oil was distilled in order
  11. 11
    Otroto obtain a yellow oil, which

Procedimiento

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).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07148173B2uspto-grants-2006_12