反应详情

温度

-78 °C

Into a one-liter Schlenk flask were placed 4.26 g of 2-dimethylaminofluorene and 250 mL of tetrahydrofuran. The flask was cooled to -78° C. Into the flask, 11 mL of a 1.72N n-BuLi solution in hexane was gradually added dropwise. The reaction solution was spontaneously brought to room temperature, and then cooled again to -78° C. Thereto, a solution of 5.1 g of diphenylfulvene in 250 mL of tetrahydrofuran was gradually added dropwise. The mixture was stirred vigorously overnight while the temperature thereof was allowed to rise spontaneously to room temperature. A red homogeneous reaction solution was thereby obtained. This reaction solution was washed with a saturated sodium chloride solution, and the solvent was evaporated off. The residue was purified by column chromatography to obtain 7.6 g of slightly yellowish white solid. This solid was placed in another Schlenk flask together with 250 mL of tetrahydrofuran. The mixture was cooled to -78° C. Thereto, 6.5 mL of a 1.72N n-BuLi solution in hexane was gradually added dropwise, and then the mixture was brought to room temperature. To this reaction solution, a solution of 1.15 g of zirconium tetrachloride in 100 mL of tetrahydrofuran was introduced slowly to obtain 1.15 g of intended diphenylmethylene(cyclopentadienyl)(2-dimethylaminofluorenyl)zirconium dichloride. This compound was identified by 1H-NMR as shown in Table 1.

1. customwas spontaneously brought to room temperature
2. temperaturecooled again to -78° C
3. customto rise spontaneously to room temperature
4. customA red homogeneous reaction solution was thereby obtained
5. washThis reaction solution was washed with a saturated sodium chloride solution
6. customthe solvent was evaporated off
7. customThe residue was purified by column chromatography
8. customto obtain 7.6 g of slightly yellowish white solid
9. temperatureThe mixture was cooled to -78° C
10. customwas brought to room temperature