反应详情

温度

0 °C

Under a nitrogen atmosphere, 0.81 g (2.20 mmol) of octamethyloctahydrodibenzofluorene and 100 ml of dehydrated tert-butyl methyl ether were added, and the mixture was stirred. This solution was cooled to 0° C., and 1.59 ml (2.42 mmol) of a 1.52 mol/l hexane solution of n-butyllithium was added. Subsequently, the mixture was stirred at room temperature for 24 hours. The resulting solution was cooled to −78° C., and 1.04 g (2 mmol) of 6,6-bis(4-(p-trifluoromethylphenyl)-phenyl)fulvene was added. The mixture was stirred at room temperature for 3 hours. When the completion of reaction was checked, 1 N hydrochloric acid was added to the reaction solution to perform liquid-liquid phase separation. The aqueous layer was subjected to extraction with diethyl ether two times, and the extract was combined with the organic layer previously obtained. The liquid was washed with a saturated aqueous solution of sodium hydrogen carbonate, water and saturated brine, and dried over magnesium sulfate. The solvent was distilled off, and the residue was subjected to separation by silica gel chromatography to obtain a target product (yield 0.92 g (47%)). The target product was identified by 1H-NMR and FD-MS spectroscopy.

1. stirringSubsequently, the mixture was stirred at room temperature for 24 hours
2. temperatureThe resulting solution was cooled to −78° C.
3. stirringThe mixture was stirred at room temperature for 3 hours
4. customWhen the completion of reaction
5. customliquid-liquid phase separation
6. extractionThe aqueous layer was subjected to extraction with diethyl ether two times
7. custompreviously obtained
8. washThe liquid was washed with a saturated aqueous solution of sodium hydrogen carbonate, water and saturated brine
9. dry with materialdried over magnesium sulfate
10. distillationThe solvent was distilled off
11. customthe residue was subjected to separation by silica gel chromatography
12. customto obtain a target product (yield 0.92 g (47%))