반응 #416882

반응 방정식

lithium dimethylamide

Zirconium tetrachloride

lithium dimethylamide

→

zirconium tetrakis(dimethylamide)

용매

diethyl ether

반응 조건

후처리

1. 1
   온도then refluxed 1 hour
2. 2
   기타All volatiles are removed under vacuum at room temperature
3. 3
   추출the remaining oily solid is extracted twice with 150 ml portions of hexane
4. 4
   기타then transferred to a 50 ml flask
5. 5
   workup.DISTILLATIONSolid zirconium tetrakis(dimethylamide) is distilled from the residue under reduced pressure (boiling point=40° C. to 60° C. @ 0.025 mm Hg)
6. 6
   기타to give a white crystalline, low melting solid

실험 절차

The lithium dimethylamide, 0.5 mole, in 250 ml of diethyl ether is chilled in an acetone/dry ice bath to -78° C. Zirconium tetrachloride, 26 g (0.112 mole), is transferred to a solid addition funnel attached to the 1000 ml Schlenk then added over 30 minutes to the magnetically stirred lithium dimethylamide slurry. The mixture is warmed slowly to room temperature then refluxed 1 hour. All volatiles are removed under vacuum at room temperature and the remaining oily solid is extracted twice with 150 ml portions of hexane. The combined extracts are reduced in solvent volume then transferred to a 50 ml flask. Solid zirconium tetrakis(dimethylamide) is distilled from the residue under reduced pressure (boiling point=40° C. to 60° C. @ 0.025 mm Hg) to give a white crystalline, low melting solid.

출처