反应详情

A 250 mL Schlenk flask is charged with toluene, 100 mL, and titanium tetrakis(diethylamide), 6.21 g (18.5 mmole). To the magnetically stirred solution is added titanium tetrachloride, 1.17 g (6.15 mmole) resulting in a gradual darkening of the solution. The mixture is stirred 1 hour while refluxing. All volatiles are removed under vacuum at room temperature leaving a yellow-brown oil. The oil is transferred to a micro distillation apparatus and distilled under vacuum. A yellow-brown liquid is obtained which distills at 112° to 118° C. (at 0.025 mm Hg). The product is determined to be chloro titanium tris(diethylamide).

1. customresulting in a gradual darkening of the solution
2. temperaturewhile refluxing
3. customAll volatiles are removed under vacuum at room temperature
4. customleaving a yellow-brown oil
5. distillationdistilled under vacuum
6. customA yellow-brown liquid is obtained which
7. distillationdistills at 112° to 118° C. (at 0.025 mm Hg)