反应详情

温度

-30 °C

Next, 0.98 g (2.11 millimole) of this 4,6-di-tert-butyl-2-diphenylphosphinophenyl trimethylsilyl ether was dissolved in 15 ml of dehydrated tetrahydrofuran under nitrogen flow, and the solution was cooled down to −30° C. Then, a dehydrated tetrahydrofuran solution of 0.4 g (1.06 millimole) of a zirconium tetrachloride tetrahydrofuran adduct was added thereto step by step, and the solution was stirred at a room temperature for one hour. Further, the solution was refluxed for 3 days by heating. The solvent was distilled off under reduced pressure, and the residue was recrystallized from dichloromethane/hexane, whereby obtained was 0.29 g (yield: 29.0%) of bis (2-diphenylphosphino-4,6-di-tert-butylphenoxy) zirconium dichloride.

1. temperatureFurther, the solution was refluxed for 3 days
2. temperatureby heating
3. distillationThe solvent was distilled off under reduced pressure
4. customthe residue was recrystallized from dichloromethane/hexane, whereby
5. customobtained