Reaktion #2295811

Reaktionsgleichung

dichlorodimethylsilane

lithium (2-methyl-4-phenylindenide)

→

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

Lösungsmittel

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto give a cloudy yellow mixture
2. 2
   SonstigeThe mixture was evaporated under vacuum
3. 3
   Sonstigeleaving a white solid
4. 4
   ExtraktionThe solid was extracted with pentane (40 mL)
5. 5
   Filtrationthe extract was filtered
6. 6
   Sonstigeto give a light yellow solution and white solid
7. 7
   SonstigeThe solution was evaporated under vacuum
8. 8
   Sonstigeleaving a white solid

Vorschrift

To a colorless solution of dichlorodimethylsilane (12.90 g, 100 mmol, 3.00 eq.) in ether (30 mL) at −30° C. was added lithium (2-methyl-4-phenylindenide) (7.07 g, 33.3 mmol, 1.00 equiv.) in portions to give a cloudy yellow mixture. The reaction was allowed to warm to room temperature and stirred for 4 hours, becoming cloudy white with precipitate. The mixture was evaporated under vacuum, leaving a white solid. The solid was extracted with pentane (40 mL) and the extract was filtered to give a light yellow solution and white solid. The solution was evaporated under vacuum, leaving a white solid. Yield 9.85 g (99%). 1H NMR (C6D6): δ 7.59 (d, 2H), 7.44 (m, IH), 7.36 (m, 3H), 7.22 (m, 2H), 6.86 (d, 1H), 3.42 (d, IH), 2.11 (d, 3H), 0.27 (s, 3H), −0.03 (s, 3H).

Quelle