Methyl iodide → HCID 178420575, Verbindung

Temperatur

23 °C

1.1 g (6.2 mMoles) of anthracene, 350 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-brown solution is formed while stirring at 23° C., orange-colored magnesium anthracene precipitating therefrom after 100 minutes. The reaction mixture is treated for about 3 hours in an ultrasonic bath (continuous peak HF output 240 watts, 35 kHz) and subsequently heated with stirring to 60° C. After the addition of 34.8 g (300 mMoles) of indene, the heat source is removed and 35.6 g (100 mMoles) of solid cobalt-(III)acetylacetonate are added over a period of 40 minutes. The reaction mixture changes color to dark brown with an increase in temperature to 68° C. After cooling to 23° C., the reaction mixture is filtered off from excess magnesium through a G-3-glass frit and the clear brown red 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 insoluble 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 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 10.3 g (35 mMoles=35.5% of the theoretical) of bis-(indenyl)-cobalt in the form of glittering black crystals.

1. customA yellow-brown 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. temperaturesubsequently heated
4. stirringwith stirring to 60° C
5. customthe heat source is removed
6. temperatureThe reaction mixture changes color to dark brown with an increase in temperature to 68° C
7. temperatureAfter cooling to 23° C.
8. filtrationthe reaction mixture is filtered off from excess magnesium through a G-3-glass frit
9. concentrationthe clear brown red filtrate is concentrated by evaporation to dryness (max. bath temperature 30° C.) in a high vacuum (10-3Torr)
10. customany insoluble fractions are isolated by filtration through a G-3-glass frit
11. washThe filter cake is washed several times with a total of 500 ml of pentane until the filtrate
12. concentrationThe clear red-brown filtrate is concentrated to approximately 200 ml
13. waitthe complex left
14. customto crystallize out at -80° C
15. customThe supernatant mother liquor is removed under pressure
16. washwashed 2 to 3 times with approximately 50 ml of pentane
17. temperaturecooled to -80° C
18. customDrying in vacuo (0.1 Torr)

ORD-Eintrag

ord-a40faf9d28d14d08a963edcb25994efa

Quelldatensatz

uspto-grants-1985_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04556719