反应详情

温度

-78 °C

A 500 mL Schlenk flask is charged with dichlorotitanium bis(dimethylamide), 7.24 g (35 mmole), and toluene, 100 mL. The mixture is stirred magnetically and chilled to -78° C. in a dry ice/acetone bath. Lithium indenide (4A-2), 45 mmole, is added to the mixture which is then allowed to warm slowly to room temperature. The mixture is stirred approximately 15 hours at room temperature. All volatiles are removed under vacuum at room temperature giving a dark viscous oil. The residue is extracted with toluene (1×50 mL) and filtered. The solution is chilled to -30° C. resulting in the formation of red/orange needles. The product is isolated by decanting the solution then vacuum drying the crystalline product. A proton NMR of the product shows it is pure indenyltitanium bis(dimethylamide) chloride. A test for chloride confirms the presence of the halide in the product.

1. temperatureto warm slowly to room temperature
2. stirringThe mixture is stirred approximately 15 hours at room temperature
3. customAll volatiles are removed under vacuum at room temperature
4. customgiving a dark viscous oil
5. extractionThe residue is extracted with toluene (1×50 mL)
6. filtrationfiltered
7. temperatureThe solution is chilled to -30° C.
8. customresulting in the formation of red/orange needles
9. customThe product is isolated
10. customby decanting the solution
11. customvacuum drying the crystalline product