反应详情

Under nitrogen atmosphere, 24.5 ml of 1.63 M hexane solution of n-butyllithium (40 mmol) was dripped down at -78° C. into 90 ml of a diethyl ether suspension of 9.37 g (40.0 mmol) of 2-i-propyl-7-phenylindene and 0.1 g (1.0 mmol) of copper (I) cyanide. After completion of the dripping, the temperature was slowly elevated to room temperature and the mixture was stirred at room temperature for 2 hours. Again, the mixture was cooled down to -78° C. and 2.58 g (20.0 mmol) of dimethyldichlorosilane was added thereto slowly. After completion of the dripping, the temperature was slowly elevated to room temperature, and the mixture was stirred for 7 hours. The reaction mixture was poured into aqueous saturated ammonium chloride solution and extracted with diethyl ether. After it was washed with saturated saline, the organic phase was dried over anhydrous magnesium sulfate, followed by distilling off the solvent to obtain viscous solids. The solids were fractionated by column chromatography (silica gel, development solvent: n-hexane) to obtain 9.69 g (18.5 mmol, yield: 92.5%) of dimethylbis(2-i-propyl-4-phenylindenyl)silane. By 1H-NMR, this was confirmed to be a mixture of two isomers.

1. customwas slowly elevated to room temperature
2. temperatureAgain, the mixture was cooled down to -78° C.
3. customwas slowly elevated to room temperature
4. stirringthe mixture was stirred for 7 hours
5. extractionextracted with diethyl ether
6. washAfter it was washed with saturated saline
7. dry with materialthe organic phase was dried over anhydrous magnesium sulfate
8. distillationby distilling off the solvent
9. customto obtain viscous solids