Reaktion #1435719

Reaktionsgleichung

potassium (2-trimethylsiloxy-ethyl)-cyclopentadienide

cyclopentadienyl zirconium trichloride

dimethoxyethane

→

cyclopentadienyl ((2-trimethylsiloxy-ethyl)-cyclopentadienyl) zirconium dichloride

Ausbeute 27.0%

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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%.

Quelle