反应详情

温度

135 °C

124 g (1 mol) of potassium methacrylate were admixed with 198.5 g (1 mol) of 3-chloropropyltrimethoxysilane, 2.7 g of 1-(3'-trimethoxysilylpropyl)-4-dimethylaminopyridinium chloride and 0.5 g of N,N'-diphenyl-p-phenylamine, and the mixture was heated to 135° C. while stirring. After 1 hour at this temperature the mixture was cooled and the potassium chloride which had precipitated was filtered off and washed with 60 g of methanol. The methanol was evaporated from the combined filtrates, and the residue was distilled under reduced pressure. 225 g of 3-methacryloxypropyltrimethoxysilane having a boiling point of 82° C. (0.4 mbar) were obtained. The yield was 90.7% of theory, based on the amount of potassium methacrylate which was used. The purity of the product was 99.0%. In the gas chromatogram only traces of 4-dimethylaminopyrrdine were detectable. A 2% solution of the product in water with a pH of 4 contained no oily separation of any kind.

1. temperatureAfter 1 hour at this temperature the mixture was cooled
2. customthe potassium chloride which had precipitated
3. filtrationwas filtered off
4. washwashed with 60 g of methanol
5. customThe methanol was evaporated from the combined filtrates
6. distillationthe residue was distilled under reduced pressure