Reaktion #672358

Reaktionsgleichung

magnesium

dichlorodimethylsilane

2-bromoindene

magnesium

1

2-chlorodimethylsilylindene

→

2-chloro-dimethyl-silylindene

Ausbeute 94.0%

Lösungsmittel

THF

—

solution

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGAfter stirring
3. 3
   Sonstigesolvent was withdrawn
4. 4
   workup.ADDITION50 ml of THF was newly added
5. 5
   workup.STIRRINGThen the solution was stirred at room temperature for 2 hours
6. 6
   workup.ADDITIONwas dropped in one hour
7. 7
   workup.STIRRINGby stirring for 15 hours
8. 8
   workup.DISTILLATIONthe solvent was distilled off
9. 9
   ExtraktionThe residue was extracted by 200 ml of hexane
10. 10
    workup.DISTILLATIONby distilling off the solvent

Vorschrift

Under nitrogen flow, 50 ml of THF (tetrahydrofuran) and 2.5 g (41 mmol) of magnesium was placed in a 1 liter 3-necked flask, to which 0.1 ml of 1 2-dibromoethane was added and stirred for 30 minutes to activate magnesium. After stirring, solvent was withdrawn and 50 ml of THF was newly added. To this, 5.0 g (25.6 mmol) of 2-bromoindene in THE (200 ml) solution was dropped in 2 hours. Then the solution was stirred at room temperature for 2 hours and cooled down to −78 ° C., to which 3.1 ml (25.6 mmol) of dichlorodimethylsilane in THF (100 ml) solution was dropped in one hour, followed by stirring for 15 hours and the solvent was distilled off. The residue was extracted by 200 ml of hexane and by distilling off the solvent, 6.6 g (24.2 mmol) of 2-chloro-dimethyl-silylindene was obtained (yield 94%).

Quelle