Reaktion #1865636

Reaktionsgleichung

chlorodimethyl(2-methyl-4-phenyl-1H-indenyl)silane

sodium (tetramethylcyclopentadienide)

→

Dimethyl(2-methyl-4-phenyl-1H-indenyl)(2,3,4,5-tetramethylcyclopentadienyl)silane

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto give a cloudy orange solution
2. 2
   SonstigeThe mixture was evaporated under vacuum
3. 3
   Sonstigeleaving an orange residue
4. 4
   ExtraktionThe residue was extracted with pentane (50 ml)
5. 5
   Filtrationthe extract was filtered
6. 6
   Sonstigeto give a bright yellow solution and yellow solid
7. 7
   SonstigeThe solution was evaporated under vacuum
8. 8
   Sonstigeto yield thick

Vorschrift

To a light yellow solution of chlorodimethyl(2-methyl-4-phenyl-1H-indenyl)silane (9.40 g, 31.4 mmol, 1.00 eq.) in tetrahydrofuran (40 ml) at −30° C. was added sodium (tetramethylcyclopentadienide) (4.76 g, 33.0 mmol, 1.05 equiv.) in portions to give a cloudy orange solution. The reaction was allowed to warm to room temperature and stirred for 23 hours. The mixture was evaporated under vacuum, leaving an orange residue. The residue was extracted with pentane (50 ml) and the extract was filtered to give a bright yellow solution and yellow solid. The solution was evaporated under vacuum to yield thick, orange oil. Yield 10.16 g (84%). 1H NMR(C6D6): δ7.61 (d, 2H), 7.41 (m, 1H), 7.31 (m, 4H), 7.19 (m, 1H), 6.85 (s, 1H), 3.60, (s, 1H), 3.16 (br s, 1H), 2.00 (s, 3H), 1.93 (s, 3H), 1.88 (s, 3H), 1.82 (s, 6H), −0.23 (s, 3H), −0.24 (s, 3H).

Quelle