dimethylazanide;zirconium(4+)

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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. then refluxed 1 hour All volatiles are removed under vacuum at room temperature the remaining oily solid is extracted twice with 150 ml portions of hexane 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

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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. then refluxed 1 hour All volatiles are removed under vacuum at room temperature the remaining oily solid is extracted twice with 150 ml portions of hexane 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

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A solution of 0.50 g of neopentyllithium in hexane was added to a hot solution of zirconium tetrakis(dimethylamide) in hot hexane with stirring. Lithium dimethylamide precipitated immediately. The total amount of hexane in the reaction mixture was about 50-100 ml. The mixture was cooled and filtered, and the filtrate was evaporated to give a sticky solid. The latter was dissolved in pentane, and the solution was kept at -40° C. for 2 days. During this time yellow crystals of neopentylzirconium tris(dimethylamide) separated. They were isolated by filtration and dried; yield 0.5 g. Nmr in C6D6 : δ (NMe) 2.92, δ (CH2) 0.9, δ (CMe3) 1.20 ppm downfield from tetramethylsilane. Lithium dimethylamide precipitated immediately The mixture was cooled filtered the filtrate was evaporated to give a sticky solid During this time yellow crystals of neopentylzirconium tris(dimethylamide) separated They were isolated by filtration dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A solution of 0.50 g of neopentyllithium in hexane was added to a hot solution of zirconium tetrakis(dimethylamide) in hot hexane with stirring. Lithium dimethylamide precipitated immediately. The total amount of hexane in the reaction mixture was about 50-100 ml. The mixture was cooled and filtered, and the filtrate was evaporated to give a sticky solid. The latter was dissolved in pentane, and the solution was kept at -40° C. for 2 days. During this time yellow crystals of neopentylzirconium tris(dimethylamide) separated. They were isolated by filtration and dried; yield 0.5 g. Nmr in C6D6 : δ (NMe) 2.92, δ (CH2) 0.9, δ (CMe3) 1.20 ppm downfield from tetramethylsilane. Lithium dimethylamide precipitated immediately The mixture was cooled filtered the filtrate was evaporated to give a sticky solid During this time yellow crystals of neopentylzirconium tris(dimethylamide) separated They were isolated by filtration dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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. then refluxed 1 hour All volatiles are removed under vacuum at room temperature the remaining oily solid is extracted twice with 150 ml portions of hexane 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

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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. then refluxed 1 hour All volatiles are removed under vacuum at room temperature the remaining oily solid is extracted twice with 150 ml portions of hexane 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

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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. then refluxed 1 hour All volatiles are removed under vacuum at room temperature the remaining oily solid is extracted twice with 150 ml portions of hexane 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

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A solution of 0.50 g of neopentyllithium in hexane was added to a hot solution of zirconium tetrakis(dimethylamide) in hot hexane with stirring. Lithium dimethylamide precipitated immediately. The total amount of hexane in the reaction mixture was about 50-100 ml. The mixture was cooled and filtered, and the filtrate was evaporated to give a sticky solid. The latter was dissolved in pentane, and the solution was kept at -40° C. for 2 days. During this time yellow crystals of neopentylzirconium tris(dimethylamide) separated. They were isolated by filtration and dried; yield 0.5 g. Nmr in C6D6 : δ (NMe) 2.92, δ (CH2) 0.9, δ (CMe3) 1.20 ppm downfield from tetramethylsilane. Lithium dimethylamide precipitated immediately The mixture was cooled filtered the filtrate was evaporated to give a sticky solid During this time yellow crystals of neopentylzirconium tris(dimethylamide) separated They were isolated by filtration dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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. then refluxed 1 hour All volatiles are removed under vacuum at room temperature the remaining oily solid is extracted twice with 150 ml portions of hexane 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