反应详情

温度

70 °C

To a solution of 20.8 g (54.1 mmol) of 4-(4-tert-butylphenyl)-6-(cyclohexylmethyl)-1,2,3,5-tetrahydro-s-indacene in 600 ml of toluene 21.7 ml (54.2 mmol) of 2.5 M nBuLi in hexanes was added dropwise at 20° C. Then, 30 ml of THF was added, and the resulting mixture was stirred for 1 h at 70° C. The resulting mixture was cooled to 0° C., and 3.30 ml (3.49 g, 27.1 mmol) of dichlorodimethylsilane was added. This mixture was stirred for 12 h at room temperature, then 5 ml of water was added, and organic solvents were evaporated using Rotavapor. The product was extracted from the residue by 3×100 ml of dichloromethane. The organic extract was dried over Na2SO4 and then evaporated to dryness. The product was isolated by flash chromatography on silica gel 60 (40-63 um, eluent: hexanes and then hexanes-dichloromethane, 10:1, vol.). Yield 15.2 g (68%).

1. temperatureThe resulting mixture was cooled to 0° C.
2. stirringThis mixture was stirred for 12 h at room temperature
3. customorganic solvents were evaporated
4. extractionThe product was extracted from the residue by 3×100 ml of dichloromethane
5. extractionThe organic extract
6. dry with materialwas dried over Na2SO4
7. customevaporated to dryness
8. customThe product was isolated by flash chromatography on silica gel 60 (40-63 um, eluent