Reaktion #806265

Reaktionsgleichung

rac-dimethylsilyl-bis (tetrahydroindenyl) zirconium dichloride

tributyltin fluoride

→

rac-dimethylsilylbis (tetrahydroindenyl) zirconium difluoride

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationwas then filtered
2. 2
   Sonstigeto give a straw-yellow solution
3. 3
   SonstigeThe solution was then evaporated in vacuo
4. 4
   Sonstigeleaving a manila-colored, thick suspension
5. 5
   WaschenThe suspension was washed with pentane (20 mL
6. 6
   Sonstige3×5 mL) to give a white, micro crystalline solid
7. 7
   SonstigeThe solid was dried in vacuo
8. 8
   Sonstigeto yield 0.76 g (82%)

Vorschrift

To a murky green-yellow solution of rac-dimethylsilyl-bis (tetrahydroindenyl) zirconium dichloride [DMS bis (THI) ZrCl2] (1.00 g, 2.19 mmol, 1.00 eq.) in dichloromethane (15 mL) was added tributyltin fluoride (1.42 g, 4.59 mmol, 2.10 eq.). The reaction lightened immediately. The reaction was stirred for one hour and was then filtered to give a straw-yellow solution and a small amount of brownish solid. The solution was then evaporated in vacuo, leaving a manila-colored, thick suspension. The suspension was washed with pentane (20 mL, then 3×5 mL) to give a white, micro crystalline solid. The solid was dried in vacuo to yield 0.76 g (82%). 1H NMR (CD2Cl2): δ 0.80 (s, 6H, SiMe2, 1.45–1.9 and 2.4–2.7 (br m, 16H, aliphatic-ring-H), 5.61 (d, 2H, cyclopentadienyl-ring-H), 6.27 (br s, 2H, cyclopentadienyl-ring-H). 19F NMR (CD2Cl2): δ 19.9 (s).

Quelle