反应详情

温度

-7.5 °C

2.4 g of butyllithium dissolved in 15 ml of hexane was slowly added during 5 minutes into 6.0 g of fluorene dissolved in 40 ml of anhydrous tetrahydrofuran at -50° C. under nitrogen protection. The mixture was stirred at -30 to 15° C. for 1 hour before it was cooled again to -40 ~-50° C. Then, 6.0 g of 1-bromohexane was added in 5 minutes. The mixture was subsequently stirred for 2 hours while the temperature was gradually increased to room temperature. The mixture was then cooled to -50° C., and 2.4 g of butyllithium dissolved in 15 ml of hexane was slowly added in 5 minutes under nitrogen protection. The mixture was stirred at -30 to 15° C. for 1 hour before it was cooled again to -40~-50° C. Then, 7.6 g of 6-bromo-2,2-dimethylhexanenitrile was added in 5 minutes. The mixture was subsequently stirred for 15 hours at room temperature, dispersed in water, and extracted with ether. The etheral solution was washed with water and brine, dried with magnesium sulfate, and evaporated. The residue was distilled to collect 12.4 g (92%) of light yellow liquid. MS (m/z): 373 (M+), 288, 249, 217, 191, 179, 165.

1. temperaturewas cooled again to -40 ~-50° C
2. stirringThe mixture was subsequently stirred for 2 hours while the temperature
3. temperaturewas gradually increased to room temperature
4. temperatureThe mixture was then cooled to -50° C.
5. additionwas slowly added in 5 minutes under nitrogen protection
6. stirringThe mixture was stirred at -30 to 15° C. for 1 hour before it
7. temperaturewas cooled again to -40~-50° C
8. stirringThe mixture was subsequently stirred for 15 hours at room temperature
9. extractionextracted with ether
10. washThe etheral solution was washed with water and brine
11. dry with materialdried with magnesium sulfate
12. customevaporated
13. distillationThe residue was distilled
14. customto collect 12.4 g (92%) of light yellow liquid