dimethylazanide;vanadium(4+)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a dark-green solution of 0.048 g (0.21 mmol) of vanadium tetrakis(dimethylamide) in hexane was added from a syringe 0.26 ml of a 1.6 M solution of butyllithium (0.21 mmol) in hexane. Lithium dimethylamide precipitated rapidly. The total volume of liquid in the mixture was about 6 ml. After 15 minutes the mixture was filtered to give a clear green solution of dibutylvanadium bis(dimethylamide) in hexane. Lithium dimethylamide precipitated rapidly After 15 minutes the mixture was filtered

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of 0.80 g of vanadium tetrakis(dimethylamide) in pentane was added a solution of 0.63 g of trimethylsilylmethyllithium in pentane. Lithium dimethylamide precipitated rapidly. The reaction mixture contained a total of about 50-100 ml of pentane. After stirring for three hours the mixture was filtered, and part of the pentane was evaporated. The solution was kept at -40° C. overnight, following which the remainder of the pentane was evaporated, to give bis(trimethylsilylmethyl)vanadium bis(dimethylamide) as a dark-green oil, which was purified by distillation at 100° C. under high vacuum. Lithium dimethylamide precipitated rapidly was filtered part of the pentane was evaporated The solution was kept at -40° C. overnight was evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of 0.80 g of vanadium tetrakis(dimethylamide) in pentane was added a solution of 0.63 g of trimethylsilylmethyllithium in pentane. Lithium dimethylamide precipitated rapidly. The reaction mixture contained a total of about 50-100 ml of pentane. After stirring for three hours the mixture was filtered, and part of the pentane was evaporated. The solution was kept at -40° C. overnight, following which the remainder of the pentane was evaporated, to give bis(trimethylsilylmethyl)vanadium bis(dimethylamide) as a dark-green oil, which was purified by distillation at 100° C. under high vacuum. Lithium dimethylamide precipitated rapidly was filtered part of the pentane was evaporated The solution was kept at -40° C. overnight was evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A small amount of vanadium tetrakis(dimethylamide) was dissolved in pentane, and an excess of trimethylsilylmethyllithium was added. Lithium dimethylamide precipitated. The mixture was filtered and the esr spectrum was recorded. An eight-line spectrum was observed at g = 1.973 ± 0.001 with a hyperfine coupling constant to vanadium of 60.3 G. This coupling constant is midway between V(NMe2)4 (65.1 G) and (Me3SiCH2)4V (55 G). This spectrum implied the existence of bis(trimethylsilylmethyl)vanadium bis(dimethylamide) in solution. Lithium dimethylamide precipitated The mixture was filtered

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a dark-green solution of 0.048 g (0.21 mmol) of vanadium tetrakis(dimethylamide) in hexane was added from a syringe 0.26 ml of a 1.6 M solution of butyllithium (0.21 mmol) in hexane. Lithium dimethylamide precipitated rapidly. The total volume of liquid in the mixture was about 6 ml. After 15 minutes the mixture was filtered to give a clear green solution of dibutylvanadium bis(dimethylamide) in hexane. Lithium dimethylamide precipitated rapidly After 15 minutes the mixture was filtered

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of 0.80 g of vanadium tetrakis(dimethylamide) in pentane was added a solution of 0.63 g of trimethylsilylmethyllithium in pentane. Lithium dimethylamide precipitated rapidly. The reaction mixture contained a total of about 50-100 ml of pentane. After stirring for three hours the mixture was filtered, and part of the pentane was evaporated. The solution was kept at -40° C. overnight, following which the remainder of the pentane was evaporated, to give bis(trimethylsilylmethyl)vanadium bis(dimethylamide) as a dark-green oil, which was purified by distillation at 100° C. under high vacuum. Lithium dimethylamide precipitated rapidly was filtered part of the pentane was evaporated The solution was kept at -40° C. overnight was evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A small amount of vanadium tetrakis(dimethylamide) was dissolved in pentane, and an excess of trimethylsilylmethyllithium was added. Lithium dimethylamide precipitated. The mixture was filtered and the esr spectrum was recorded. An eight-line spectrum was observed at g = 1.973 ± 0.001 with a hyperfine coupling constant to vanadium of 60.3 G. This coupling constant is midway between V(NMe2)4 (65.1 G) and (Me3SiCH2)4V (55 G). This spectrum implied the existence of bis(trimethylsilylmethyl)vanadium bis(dimethylamide) in solution. Lithium dimethylamide precipitated The mixture was filtered