Dichlorodimethylsilane → HCID 59735669, Verbindung

HRID 2425313Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2425313
[Li]CCCC.[CH3:6][C:7]1[CH2:8][C:9]2[C:14]([CH:15]=1)=[C:13]([CH3:16])[CH:12]=[C:11]([CH3:17])[CH:10]=2.[Si:18]([CH3:22])([CH3:21])(Cl)[Cl:19].[Li]>CCCCCC.CCOCC.C1COCC1>[Cl:19][Si:18]([CH:8]1[C:9]2[C:14](=[C:13]([CH3:16])[CH:12]=[C:11]([CH3:17])[CH:10]=2)[CH:15]=[C:7]1[CH3:6])([CH3:22])[CH3:21]

Komponenten

8

Edukt 4

HCID 6398DichlorodimethylsilaneHCID 3028194LithiumHCID 109207862,4,6-trimethyl-1H-indeneHCID 178418339Butyllithium

Produkt 1

HCID 59735669HCID 59735669, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 8058HexaneLösungsmittel

Versuchsvorschrift

A 2.5 M n-BuLi solution in hexane (9.6 mL) was added dropwise at 0° C. under nitrogen to a solution of 3.6 g of 2,4,6-trimethylindene in 35 mL of Et2O. During the addition a white-off suspension was formed. After 10 min the mixture was allowed to warm up to r.t. and stirred for 30 min, with final formation of a white suspension. Then a solution of Me2SiCl2 (4 mL) in 35 mL of THF was cooled to 0° C. and slowly added to the lithium salt suspension, also cooled to 0° C. After 30 min the yellow reaction mixture was allowed to warm up to r.t. and stirred for 24 h. Then the solvents were removed in vacuo and the light orange oil with a powder was characterized by 1H-NMR spectroscopy. The product was used as such in the next step without further purification.

Aufarbeitung

  1. additionDuring the addition a white-off suspension
  2. customwas formed
  3. temperaturealso cooled to 0° C
  4. waitAfter 30 min the yellow reaction mixture was allowed
  5. temperatureto warm up to r.t.
  6. stirringstirred for 24 h
  7. customThen the solvents were removed in vacuo
  8. customwithout further purification

Quellen und Nachweise

ORD-Eintrag
ord-2f07651d63e64255823baeb08801fae1
Quelldatensatz
uspto-grants-2011_06
Patentnummer
US07964679B2

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