反应详情

温度

-78 °C

In a first reaction step, 3-aminopropyltriethoxysilane (159.39 g, 0.72 mol, 1.00 eq) is initially charged in ethanol (3.0 l) in a 4 l three-neck flask with precision glass stirrer, internal thermometer, dropping funnel and reflux condenser, and cooled to −78° C. 2-Chloroethyl isocyanate (75.92 g, 0.72 mol, 1.00 eq) is added dropwise at −78 to −69° C. within 2.25 h and then the mixture is heated to 50° C. Dry sodium sulphide (Na2S, 28.09 g, 0.36 mol, 0.50 eq) is added in five portions and the mixture is heated to reflux. After a reaction time of 4.5 h, the mixture is cooled to room temperature and the suspension is filtered. The filtrate is freed of the solvent on a rotary evaporator and dried under reduced pressure. The (EtO)3Si—CH2CH2CH2—NH—CO—NH—CH2CH2—S—CH2CH2—NH—CO—NH—CH2CH2CH2—Si(OEt)3 product (214.09 g, 96.7% of theory) is obtained as a waxy, white solid.

1. temperaturereflux condenser
2. temperaturethe mixture is heated to 50° C
3. temperaturethe mixture is heated to reflux
4. temperatureAfter a reaction time of 4.5 h, the mixture is cooled to room temperature
5. filtrationthe suspension is filtered
6. customThe filtrate is freed of the solvent on a rotary evaporator
7. customdried under reduced pressure