反应详情

温度

-20 °C

To a solution of 10.5 g (30.0 mmol) of 5-tert-butyl-7-(4-tert-butylphenyl)-6-methoxy-2-methyl-1H-indene in 200 ml of toluene 12.0 ml (30.0 mmol) of 2.5 M nBuLi in hexanes was added at room temperature. The resulting viscous solution was stirred for 10 h, and then 10 ml of THF was added. The formed mixture was stirred for 2 h at 60° C., then cooled to −20° C., and 19.4 g (150 mmol, 5 eq.) of dichlorodimethylsilane was added in one portion. The resulting solution was warmed to room temperature, refluxed for 1 h, and then filtered through glass frit (G3). The precipitate was additionally washed by 2×10 ml of toluene. The combined filtrate was evaporated to dryness to give 13.2 g (99%) of the title product as a yellowish oil which was further used without an additional purification.

1. stirringThe formed mixture was stirred for 2 h at 60° C.
2. temperatureThe resulting solution was warmed to room temperature
3. temperaturerefluxed for 1 h
4. filtrationfiltered through glass frit (G3)
5. washThe precipitate was additionally washed by 2×10 ml of toluene
6. customThe combined filtrate was evaporated to dryness