反应详情

温度

-78 °C

The same apparatus described in Step (1) of Example B is used in this procedure. The 250 mL dropping funnel is charged with 50 mL of toluene and titanium tetrachloride, 7.7 mL (75 mmole), and added to the solution of lithium diethylamide which is chilled to -78° C. over the course of 30 minutes. The mixture is warmed to room temperature then refluxed two hours. All volatiles are removed under vacuum and the residue is extracted twice with 100 mL portions of hexane and filtered from the lithium salts. The combined extracts are reduced in solvent volume then transferred to a small scale distillation apparatus. The complex titanium tetrakis(diethylamide) is distilled from the mixture at 103°-105° C. (0.025 mm Hg) to give approximately 8 g as an orange liquid.

1. temperatureThe mixture is warmed to room temperature
2. temperaturethen refluxed two hours
3. customAll volatiles are removed under vacuum
4. extractionthe residue is extracted twice with 100 mL portions of hexane
5. filtrationfiltered from the lithium salts
6. distillationthen transferred to a small scale distillation apparatus
7. distillationThe complex titanium tetrakis(diethylamide) is distilled from the mixture at 103°-105° C. (0.025 mm Hg)
8. customto give approximately 8 g as an orange liquid