反应详情

温度

-78 °C

A 250 mL Schlenk flask is charged with indenyltitanium bis(diethylamide) chloride, 1 g (2.92 mmole), and diethylether, 100 mL. The mixture is chilled to -78° C. in a dry ice acetone bath and stirred magentically. The lithium di-n-propylamide prepared in Example 4D, step 1, is added to the flask via cannula. The mixture is slowly warmed to room temperature while stirring. The mixture is then refluxed approximately 2 hours. All volatiles are removed under vacuum at room temperature leaving a deeply colored yellow-brown, viscous oil. The residue is placed under high vacuum, 1×10-6Torr, for a few hours in order to remove any unreacted indene. Chloride analysis and NMR indicate the product is sufficiently pure indenyltitanium bis(diethylamide) di-n-propylamide, IX, and is used without further purification.

1. temperatureThe mixture is slowly warmed to room temperature
2. stirringwhile stirring
3. temperatureThe mixture is then refluxed approximately 2 hours
4. customAll volatiles are removed under vacuum at room temperature
5. customleaving a deeply colored yellow-brown, viscous oil
6. waitThe residue is placed under high vacuum, 1×10-6Torr, for a few hours in order
7. customto remove any unreacted indene
8. customis used without further purification