反应详情

A 250 mL Schlenk flask is charged with titanium tetrakis(dimethylamide), 2.48 g (11.06 mmole), and toluene, 100 mL. Freshly cracked cyclopentadiene monomer, 2.7 mL (33.18 mmole), is added to the magnetically stirred solution. The mixture is refluxed 1 hour giving a deep red solution. All volatiles are removed under vacuum at room temperature leaving a viscous deep red oil. The oil is transferred to a microdistillation apparatus and a low melting solid is distilled at 70° C. under vacuum (0.05 mm Hg). The product is determined to be cyclopentadienyltitanium tris(dimethylamide).

1. temperatureThe mixture is refluxed 1 hour
2. customgiving a deep red solution
3. customAll volatiles are removed under vacuum at room temperature
4. customleaving a viscous deep red oil
5. distillationa low melting solid is distilled at 70° C. under vacuum (0.05 mm Hg)