反应详情

To solution of 1-phenylnaphthalen-2-ol (2.0 g, 9.1 mmol) in toluene (100 mL), slowly injected was n-butyllithium (2.5 M in hexane, 3.6 mL) at −78° C., and the mixture was stirred at ambient temperature for 12 hours. After chilling the reaction mixture to −78° C., slowly added was solution of (pentamethylcyclopentadienyl)titanium(IV) trichloride (2.5 g, 16.3 mmol) in toluene (60 mL), and the reaction was carried out at ambient temperature for 12 hours. When the reaction was completed, the reaction mixture was filtered through a celite filter, and solvent was removed therefrom. Recrystallization was carried out from purified toluene and hexane at −35° C. The solid was filtered and dried under reduced pressure to obtain (dichloro)(pentamethylcyclopentadienyl)(1-phenylnaphthalen-2-yloxy)titanium(IV) (2.5 g, yield: 58.2%) as red solid.

1. customat −78° C.
2. temperatureAfter chilling the reaction mixture to −78° C.
3. additionslowly added
4. waitthe reaction was carried out at ambient temperature for 12 hours
5. filtrationthe reaction mixture was filtered through a celite
6. filtrationfilter
7. customsolvent was removed
8. customRecrystallization
9. customfrom purified toluene and hexane at −35° C
10. filtrationThe solid was filtered
11. customdried under reduced pressure