反应详情

The same apparatus described in Step (1) of Example C is used in this procedure. The 250 mL dropping funnel is charged with toluene, 100 mL, and titanium tetrachloride, 10.7 g (0.0562 mole). This is added dropwise to the flask containing lithium di-n-propylamide while stirring magnetically. Total additions times are typically 30 minutes. The mixture is refluxed for 1.5 hours. All volatiles are removed by distillation and under vacuum to give a deeply colored brown, oily residue. The residue is extracted with hexane, 2×150 mL, then filtered from the lithium salts. The extracts are combined and solvent is removed under vacuum. The remaining oil is transferred to a small scale distillation apparatus. Vacuum distillation at 157° C. and 0.05 mm Hg gave the product as an orange-brown liquid, titanium tetrakis(dipropylamide).

1. additionThis is added dropwise to the flask
2. temperatureThe mixture is refluxed for 1.5 hours
3. customAll volatiles are removed by distillation and under vacuum
4. customto give a deeply colored brown, oily residue
5. extractionThe residue is extracted with hexane, 2×150 mL
6. filtrationfiltered from the lithium salts
7. customsolvent is removed under vacuum
8. distillationThe remaining oil is transferred to a small scale distillation apparatus
9. distillationVacuum distillation at 157° C.