反应详情

温度

-78 °C

There was dissolved 3.00 g (9.42 mmol) of 2,7-diphenylfluorene in 60 mL of THF, and the obtained solution was cooled down to −78° C. To the solution, 6.12 mL of a 1.54 M-concentration hexane solution of n-butyllithium was added slowly, 6.12 mL of said hexane solution containing 9.42 mmol of n-butyllithium. Temperature of the resultant mixture was raised up to a room temperature, and the mixture was stirred for 2 hours at a room temperature. The mixture was cooled down to −78° C., and a solution of 3.06 g (9.42 mmol) of (2-allyloxy-3-tert-butyl-5-methylphenyl)chlorodiethylsilane in 14 mL of toluene was added to the mixture. Temperature of the resultant mixture was raised up to a room temperature, and the mixture was stirred for 3 hours, thereby obtaining a reaction solution. A mixture of 50 mL of a 10% aqueous solution of sodium hydrogen carbonate and 50 mL of a 10% aqueous solution of sodium carbonate was added to the reaction solution at 0° C. To the obtained mixture, 58 mL of toluene was added, and the mixture was separated to the toluene solution and the aqueous solution. The toluene solution was dried over sodium sulfate, and the mixture was filtered. The obtained filtrate was concentrated under a reduced pressure. A small amount of toluene was added the concentrated filtrate to obtain a solution, and hexane was further added thereto, thereby obtaining 3.66 g (yield: 64.0%) of (2-allyloxy-3-tert-butyl-5-methylphenyl)(2,7-diphenyl fluoren-9-yl)diethylsilane as a white solid.

1. concentrationTo the solution, 6.12 mL of a 1.54 M-concentration hexane solution of n-butyllithium
2. additionwas added slowly
3. temperatureThe mixture was cooled down to −78° C.
4. stirringthe mixture was stirred for 3 hours
5. customobtaining a reaction solution
6. additionwas added to the reaction solution at 0° C
7. customthe mixture was separated to the toluene solution
8. dry with materialThe toluene solution was dried over sodium sulfate
9. filtrationthe mixture was filtered
10. concentrationThe obtained filtrate was concentrated under a reduced pressure
11. additionA small amount of toluene was added the concentrated filtrate
12. customto obtain a solution, and hexane
13. additionwas further added