Reaktion #2041133

Reaktionsgleichung

lithium chloride

n-butyllithium

2-methyl-7-phenylindene

dimethyldichlorosilane

→

dimethyl(2-methyl-4-phenylindenyl)silyl chloride

Lösungsmittel

diethyl ether

hexane

THF

n-hexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigedried over Na-K alloy), to which
2. 2
   workup.ADDITIONwas added a solution of 2-methyl-7-phenylindenyllithium (i.e.
3. 3
   Sonstigeprecipitated
4. 4
   Extraktionthe supernatant was extracted with a syringe
5. 5
   Sonstigetransferred into another flask
6. 6
   workup.DISTILLATIONlow boiling components (solvent and unreacted dimethyidichlorosilane) were distilled off under reduced pressure at 8 mmHg

Vorschrift

23 g (180 mmol) of dimethyldichlorosilane was dissolved in 200 ml of dry n-hexane (dried over Na-K alloy), to which was added a solution of 2-methyl-7-phenylindenyllithium (i.e., a solution of 7.4 g (36 mmol) of 2-methyl-7-phenylindene in 70 ml of dry diethyl ether to which was dripped down 22.5 ml of a 1.6 M hexane solution of n-butyllithium at -78° C., followed by stirring at room temperature for 3 hours and by addition of 50 ml of THF) under ice cooling. The mixture was stirred as was at room temperature for 3 hours to deposit white salt of lithium chloride. After standing the mixture so that the white salt precipitated, the supernatant was extracted with a syringe and transferred into another flask and low boiling components (solvent and unreacted dimethyidichlorosilane) were distilled off under reduced pressure at 8 mmHg to obtain dimethyl(2-methyl-4-phenylindenyl)silyl chloride.

Quelle