4-bromobutyl-chloro-dimethylsilane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Hexachloroplatinic acid hexahydrate (0.02 g, 0.039 mmole) was dissolved in a minimum of 2-propanol. This solution was dissolved in 75 ml toluene under argon. 2-propanol and water were removed by azeotropically distilling 25 ml of the toluene. The resulting solution was stirred and 6.17 g (0.046 mole) of 4-bromo-1-butene was added at 40° C. 4.32 g (0.046 mole) of dimethylchlorosilane was slowly added and the solution was heated to 60° C. and allowed to react for four hours. The mixture was distilled to remove the toluene. Further vacuum distillation yielded 8.0 g of product with a b.p. of 92°-95° C. at 5 mm Hg pressure. 'H NMR confirmed the structure. 2-propanol and water were removed by azeotropically distilling 25 ml of the toluene to react for four hours The mixture was distilled to remove the toluene Further vacuum distillation

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This novel monomer was synthesized by adding 6.7 g (0.029 mole) of 4-bromobutyldimethylchlorosilane dropwise at 0° C. to a stirred solution of propynyllithium (1.34 g, 0.029 mole) in 50 ml of dry diethyl ether. The reaction mixture was stirred overnight at 25° C. and then poured into 400 ml of ice water. The ether layer was washed with distilled water, separated, and dried over MgSO4. The ether layer was then filtered and the product separated by removing the ether using a rotovapor. The resulting oil was purified by vacuum distillation and had a b.p. of 70°-75° C. at 15 mm Hg pressure. Yield was 75% of theoretical. 'H NMR confirmed the structure. This novel monomer was synthesized The ether layer was washed with distilled water separated dried over MgSO4 The ether layer was then filtered the product separated by removing the ether using a rotovapor The resulting oil was purified by vacuum distillation