Reaktion #928293

ord-cf7da4c08a8b49a2ab659941f2df4ca2

Lösungsmittel

Reaktionsbedingungen

Temperatur
-78°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter addition
  2. 2
    Sonstigethe cooling bath was removed
  3. 3
    SonstigeVolatiles were removed under vacuum at room temperature
  4. 4
    Extraktionthe residue was extracted twice with hexanes (2×20 mL)
  5. 5
    Sonstigethe solvent was removed under vacuum

Vorschrift

(2,3,4,5-Tetramethylcyclopentadienyl)lithium (1.33 g, 10.37 mmol) was dissolved in 80 mL THF and cooled to −78° C., and MeSiCl3 (1.70 g, 11.4 mmol) was added via a syringe. After addition, the cooling bath was removed and the reaction mixture was stirred at room temperature for 16 h. Volatiles were removed under vacuum at room temperature, and the residue was extracted twice with hexanes (2×20 mL). The hexane fractions were combined and the solvent was removed under vacuum to give a pale yellow oil (tetramethylcyclopentadienyl methyl silicon dichloride); 2.0 g, 82% yield. 1H-NMR (C6D6): δ (ppm): 2.95 (broad s, 1 H; Me4CpH), 1.92 (s, 6H;), 1.63 (s, 6H; Me4Cp), 0.19 (s, 3 H; MeSi).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06369253B1uspto-grants-2002_04