반응 #672358

반응 방정식

magnesium

dichlorodimethylsilane

2-bromoindene

magnesium

1

2-chlorodimethylsilylindene

→

2-chloro-dimethyl-silylindene

수율 94.0%

용매

THF

—

solution

THF

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGAfter stirring
3. 3
   기타solvent was withdrawn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
   추출The residue was extracted by 200 ml of hexane
10. 10
    workup.DISTILLATIONby distilling off the solvent

실험 절차

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 After stirring, solvent was withdrawn and 50 ml of THF was newly added.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%).

출처