Реакция #1435719

ord-1300e5691eec40cbacbf276870028817

Уравнение реакции

C[Si](C)(C)OCC[c-]1cccc1.[K+]
potassium (2-trimethylsiloxy-ethyl)-cyclopentadienide
[Cl-].[Cl-].[Cl-].[Zr+3][CH]1C=CC=C1
cyclopentadienyl zirconium trichloride
COCCOC
dimethoxyethane
C[Si](C)(C)OCC[C]1([Zr+2][CH]2C=CC=C2)C=CC=C1.[Cl-].[Cl-]
cyclopentadienyl ((2-trimethylsiloxy-ethyl)-cyclopentadienyl) zirconium dichloride
Выход 27.0%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONis added
  2. 2
    workup.ADDITIONThe addition
  3. 3
    Другоеis carried out at −78° C
  4. 4
    ДругоеAn orange-brown suspension is immediately formed
  5. 5
    Температураit is maintained
  6. 6
    workup.WAITthen it is left
  7. 7
    Фильтрацияit is filtered
  8. 8
    КонцентрированиеThe obtained orange solution is concentrated up to 5 ml and hexane
  9. 9
    workup.ADDITIONis added, so that a brown solid
  10. 10
    Другоеis obtained

Методика

To a suspension of 3.52 g (10 mmol) of an adduct of cyclopentadienyl zirconium trichloride with dimethoxyethane in toluene, a suspension of 2.2 g (10 mmol) of potassium (2-trimethylsiloxy-ethyl)-cyclopentadienide in toluene is added. The addition is carried out at −78° C. An orange-brown suspension is immediately formed; it is maintained under stirring for 12 hours; then it is left settling and it is filtered. The obtained orange solution is concentrated up to 5 ml and hexane is added, so that a brown solid is obtained. (1.1 g, 2.7 mmol. Yield: 27%). 1H-NMR: 6.00 (t, 2H), 5.87 (s, 5H), 5.67 (t, 2H), 3.66 (t, 2H), 2.92 (t, 2H), 0.11 (s, 9H). Mass spectrum. M+-65: (343): 33%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07211538B2uspto-grants-2007_05