反应详情

温度

20 °C

1.1 g (6.2 mMoles) of anthracene, 300 ml of THF and 0.1 ml of methyliodide are added to 14.4 g (600 mMoles) of magnesium powder (particle size <0.15 mm) in an inert gas atmosphere. A yellow-green solution is formed with stirring at 20° C., orange-colored magnesium anthracene precipitating therefrom after about 2 hours. The reaction mixture is treated for about 3 hours in an ultrasonic bath (continuous peak HF output 240 watts, 35 kHz) and then heated with stirring to 60° C. After the addition of 19.8 g (300 mMoles) of monomeric cyclopentadiene, the heat source is removed and 35.6 g (100 mMoles) of solid cobalt-(III)acetyl acetonate are added over a period of 20 minutes. The reaction mixture changes color to dark brown with vigorous evolution of heat and begins refluxing (66° C.). After cooling to 20° C., the reaction mixture is filtered off from unreacted magnesium through a G-3-glass frit and the clear dark brown filtrate is concentrated by evaporation to dryness (max. bath temperature 30° C.) in a high vacuum (10-3Torr). The residue is taken up in 500 ml of pentane and any undissolved fractions are isolated by filtration through a G-3-glass frit. The filter cake is washed several times with a total of 500 ml of pentane until the filtrate is substantially colorless. The clear red-brown filtrate is concentrated to approximately 200 ml and the complex is left to crystallize out at -80° C. The supernatant mother liquor is removed under pressure and washed 2 to 3 times with approximately 50 ml of pentane cooled to -80° C. Drying in vacuo (0.1 Torr) gives 12.4 g (63.7 mMoles=63.7% of the theoretical) of pure cobaltocene in the form of black-violet crystals melting at 172.5° C., as measured in an inert gas atmosphere.

1. customA yellow-green solution is formed
2. additionThe reaction mixture is treated for about 3 hours in an ultrasonic bath (continuous peak HF output 240 watts, 35 kHz)
3. temperatureheated
4. stirringwith stirring to 60° C
5. customthe heat source is removed
6. temperatureThe reaction mixture changes color to dark brown with vigorous evolution of heat
7. temperaturebegins refluxing (66° C.)
8. temperatureAfter cooling to 20° C.
9. filtrationthe reaction mixture is filtered off from unreacted magnesium through a G-3-glass frit
10. concentrationthe clear dark brown filtrate is concentrated by evaporation to dryness (max. bath temperature 30° C.) in a high vacuum (10-3Torr)
11. customany undissolved fractions are isolated by filtration through a G-3-glass frit
12. washThe filter cake is washed several times with a total of 500 ml of pentane until the filtrate
13. concentrationThe clear red-brown filtrate is concentrated to approximately 200 ml
14. waitthe complex is left
15. customto crystallize out at -80° C
16. customThe supernatant mother liquor is removed under pressure
17. washwashed 2 to 3 times with approximately 50 ml of pentane
18. temperaturecooled to -80° C
19. customDrying in vacuo (0.1 Torr)