Reaktion #2303898

Reaktionsgleichung

n-BuLi

hexane

2-methyl-4-phenyl-indene

dichlorodimethylsilane

→

straw yellow solid

Ausbeute 92.8%

chloro(2-methyl-4-phenyl-1-indenyl)dimethylsilane

Ausbeute 92.8%

Lösungsmittel

ether

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThis solution was cooled again to 0° C.
2. 2
   Temperaturto warm to room temperature
3. 3
   workup.STIRRINGstirred for 1 h
4. 4
   EinengenThe final straw yellow suspension was concentrated under vacuum
5. 5
   Extraktionthe residue was extracted with 50 mL of toluene
6. 6
   SonstigeThe extract was dried under vacuum

Vorschrift

A 2.5 M solution of n-BuLi in hexane (4.85 mL, 12.12 mmol) was added at 0° C. to a solution of 2.50 g of 2-methyl-4-phenyl-indene (Boulder Scientific Company, Mw=206.29, 12.12 mmol, n-BuLi:2-Me-4-Ph-Ind=1:1) in 30 mL of ether. The resulting mixture was stirred for additional 2 h at room temperature with final formation of an orange solution. This solution was cooled again to 0° C. and added slowly of a solution of 1.58 mL of dichlorodimethylsilane (Aldrich, Mw=129.06, d=1.064, 13.03 mmol, Me2SiCl2:2-Me-4-Ph-Ind=1.08:1) in 20 mL of ether. The reaction mixture was then allowed to warm to room temperature and stirred for 1 h. The final straw yellow suspension was concentrated under vacuum and the residue was extracted with 50 mL of toluene. The extract was dried under vacuum to give 3.36 g of a straw yellow solid, which was characterized by GC-MS analysis and 1H-NMR spectroscopy. Yield=92.8%.

Quelle