反应详情

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.

1. customLithium dimethylamide precipitated immediately
2. temperatureThe mixture was cooled
3. filtrationfiltered
4. customthe filtrate was evaporated
5. customto give a sticky solid
6. customDuring this time yellow crystals of neopentylzirconium tris(dimethylamide) separated
7. customThey were isolated by filtration
8. customdried