反应详情

Under an inert gas, 24.2 g magnesium chips (1.0 mol) were combined with about 20 ml methyl-tert-butylether, an iodine crystal and 3.1 g 2-chloropropane (0.04 mol). To start the reaction a solution of 61.9 g tetramethoxysilane (0.41 mol) and 75.4 g 2-chloropropane (0.96 mol) in 140 ml methyl-tert-butylether was added dropwise, with stirring, to the first mixture at a rate to maintain a moderate reflux. After addition of the solution, the reaction was allowed to reflux for six more hours. After cooling the reaction mixture, 6.0 g methanol (0.19 mol) was added, the mixture was stirred for a few minutes and then the resulting precipitate was removed by filtration. After washing the filter cake with several portions of methyl-tert-butylether, the solvent was distilled from the combined filtrates. The remaining residue consisted of 70.5 g diisopropyldimethoxysilane (98% of the theoretical yield) which had a purity of 98% according to GC. Triisopropylmethoxysilane was not detected by GC.

1. additionwas added dropwise
2. temperatureto maintain a moderate reflux
3. additionAfter addition of the solution
4. temperatureto reflux for six more hours
5. additionwas added
6. stirringthe mixture was stirred for a few minutes
7. customthe resulting precipitate was removed by filtration
8. washAfter washing the filter cake with several portions of methyl-tert-butylether
9. distillationthe solvent was distilled from the combined filtrates
10. customtheoretical yield) which