反应详情

To a stirred solution of 4.20 g of titanium tetrakis(dimethylamide) in about 10 ml of pentane was added a solution of 1.77 g of trimethylsilylmethyllithium in pentane. Lithium dimethylamide precipitated immediately. The mixture was stirred for 1 hour and filtered, pentane was removed from the filtrate by rotary evaporation, and the residual pale-yellow oil was distilled through a short still-head under reduced pressure, to give 0.87 g of trimethylsilylmethyltitanium tris(dimethylamide), bp 55° C. (50 μ). Nmr in C6D6 : δ (NMe) 3.07, δ (SiMe) 0.22, δ (CH2) 0.35 ppm downfield from tetramethylsilane.

1. customLithium dimethylamide precipitated immediately
2. filtrationfiltered
3. custompentane was removed from the filtrate by rotary evaporation
4. distillationthe residual pale-yellow oil was distilled through a short still-head under reduced pressure