反应详情

温度

-10 °C

70 ml (0.175 moles) of lithium butyl 2.5M in hexane are added, over a period of about 20 minutes, to a solution of 25 g (0.215 moles) of indene in 100 ml of tetrahydrofuran. The mixture is left under stirring for 2 hours, and is then cooled to -10° C. 20 g (0.076 moles) of α,α'-dibromo-o-xylene dissolved in 100 ml of THF are then added, in about 1 hour, so that the temperature of the reaction mixture does not exceed -5° C. At the end, the temperature is left to rise to room temperature, the mixture is hydrolyzed with water and extracted with ethyl ether. The ether extracts, after washing until neutral, and drying on anhydrous sodium sulfate, are evaporated. The residue obtained is purified on a silica gel column using petroleum ether containing 1% of ethyl acetate as eluant. After evaporation of the eluant, 9.5 g of α,α'-bis(1-indenyl)-o-xylene, are obtained, characterized by 1H-NMR analysis, with a yield of 26% with respect to the starting dibromo-o-xylene.

1. waitThe mixture is left
2. additionare then added, in about 1 hour, so that the temperature of the reaction mixture
3. customdoes not exceed -5° C
4. waitAt the end, the temperature is left
5. customto rise to room temperature
6. extractionextracted with ethyl ether
7. washafter washing until neutral, and
8. dry with materialdrying on anhydrous sodium sulfate
9. customare evaporated
10. customThe residue obtained
11. customis purified on a silica gel column
12. customAfter evaporation of the eluant, 9.5 g of α,α'-bis(1-indenyl)-o-xylene
13. customare obtained