乙氧基二甲基氯甲基硅烷

反应条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 500 ml three-necked flask having a reflux condenser, KPG stirrer and thermometer, 317 g of dry cyclohexylamine were heated to 130° C., and 122 g of (chloromethyl)ethoxydimethylsilane were added in the course of 45 min with stirring. After the end of the addition, stirring was effected for a further 30 min at 130° C. and excess cyclohexylamine was distilled off under reduced pressure. Thereafter, the mixture was cooled to 30° C. and 150 ml of isohexane were added. Thereafter, the suspension was filtered using a pressure filter, and the precipitate was rinsed with two 80 ml portions of isohexane. Filtrate and wash solutions were combined and were freed from the solvent under reduced pressure. The subsequent fractional distillation gave 163 g (yield 95%) of (N-cyclohexyl-aminomethyl)ethoxydimethylsilane with a chloride content of <20 ppm. When 1% of ammonia was added before the distillation of the product and any precipitate which separated out was filtered off, a product having a chloride content of <10 ppm was obtained in the same yield. In a 500 ml three-necked flask having After the end of the addition stirring excess cyclohexylamine was distilled off under reduced pressure 150 ml of isohexane were added Thereafter, the suspension was filtered filter the precipitate was rinsed with two 80 ml portions of isohexane Filtrate and wash solutions The subsequent fractional distillation

反应条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 500 ml three-necked flask having a reflux condenser, KPG stirrer and thermometer, 176 g of commercial cyclohexylamine (water content ≦2%) were heated to 100° C., and 122 g of (chloromethyl)ethoxydimethylsilane were added over the course of 30 min with stirring. After the end of the addition, the mixture was stirred for two hours under reflux and cooled to 30° C., and the white precipitate formed was filtered using a pressure filter, and rinsed with cyclohexylamine. Filtrate and wash solutions were combined and were freed from excess cyclohexylamine under reduced pressure. The subsequent fractional distillation gave 105 g (yield 61%) of (N-cyclohexylaminomethyl)ethoxydimethylsilane having a chloride content of 600 ppm. In a 500 ml three-necked flask having After the end of the addition the mixture was stirred for two hours under reflux the white precipitate formed was filtered filter rinsed with cyclohexylamine Filtrate and wash solutions The subsequent fractional distillation

反应条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 500 ml three-necked flask having a reflux condenser, KPG stirrer and thermometer, 176 g of commercial cyclohexylamine (water content ≦2%) were heated to 100° C., and 122 g of (chloromethyl)ethoxydimethylsilane were added over the course of 30 min with stirring. After the end of the addition, the mixture was stirred for two hours under reflux and cooled to 30° C., and the white precipitate formed was filtered using a pressure filter, and rinsed with cyclohexylamine. Filtrate and wash solutions were combined and were freed from excess cyclohexylamine under reduced pressure. The subsequent fractional distillation gave 105 g (yield 61%) of (N-cyclohexylaminomethyl)ethoxydimethylsilane having a chloride content of 600 ppm. In a 500 ml three-necked flask having After the end of the addition the mixture was stirred for two hours under reflux the white precipitate formed was filtered filter rinsed with cyclohexylamine Filtrate and wash solutions The subsequent fractional distillation