反应详情

温度

80 °C

8.0 g (61.4 mmoles) of 2-methylindene were introduced into 175 mL of toluene and 13 mL of THF, and 24.6 mL of n-butyllithium (2.5 M in toluene) were added without interruption at room temperature. After this addition was complete, the mixture was heated to 80° C. and stirred at this temperature for one hour. It was allowed to cool to 40° C., then 3.96 g (30.7 mmoles) of dimethyldichlorosilane were slowly added dropwise. After this addition, the reaction solution was stirred for three hours at 60° C. and then overnight at room temperature. 70 mL of water were added and the phases that form were separated. The organic phase was washed with 100 mL of water, and the aqueous phase was extracted three times with a total of 100 mL of toluene. The combined organic phases were dried over magnesium sulfate. After separation of the magnesium sulfate, the solvent was removed and the residue was purified by column chromatography. The desired product was isolated in a yield of 8.16 g (84%) (purity 99%).

1. additionwere added without interruption at room temperature
2. additionAfter this addition
3. temperatureto cool to 40° C.
4. additionAfter this addition
5. stirringthe reaction solution was stirred for three hours at 60° C.
6. customovernight
7. customat room temperature
8. customthe phases that form were separated
9. washThe organic phase was washed with 100 mL of water
10. extractionthe aqueous phase was extracted three times with a total of 100 mL of toluene
11. dry with materialThe combined organic phases were dried over magnesium sulfate
12. customAfter separation of the magnesium sulfate
13. customthe solvent was removed
14. customthe residue was purified by column chromatography