反应详情

温度

-20 °C

To a solution of 15.7 g (38.8 mmol) of 5-tert-butyl-7-(3,5-di-tert-butylphenyl)-6-methoxy-2-methyl-1H-indene in 200 ml of toluene 16.0 ml (40.0 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. This mixture was stirred for 2 h at 60° C., then cooled to −20° C., and 25.0 g (194 mmol, 5 eq.) of dichlorodimethylsilane was added in one portion. The resulting solution was refluxed for 2 h, then evaporated to ca. ¾ of its volume, and filtered through glass frit (G3). The precipitate was additionally washed by 2×30 ml of toluene. The combined filtrate was evaporated to dryness to give 19.2 g (99%) of white solid which was further used without an additional purification.

1. stirringThis mixture was stirred for 2 h at 60° C.
2. temperatureThe resulting solution was refluxed for 2 h
3. customevaporated to ca. ¾ of its volume
4. filtrationfiltered through glass frit (G3)
5. washThe precipitate was additionally washed by 2×30 ml of toluene
6. customThe combined filtrate was evaporated to dryness