反应详情

温度

-78 °C

3-Aminopropyltriethoxysilane (132.82 g, 0.60 mol, 1.00 eq) is initially charged in ethanol (300 ml) in a three-neck flask with precision glass stirrer, internal thermometer, dropping funnel and reflux condenser, and cooled to −78° C. 2-Chloroethyl isocyanate (63.34 g, 0.60 mol, 1.00 eq) is added dropwise at −78 to −68° C. within 1.75 h and then the mixture is heated to 50° C. Potassium thioacetate (68.53 g, 0.60 mol, 1.00 eq) is added in five portions and the mixture is heated to reflux. After a reaction time of 2.25 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—CH3 product (213.91 g, 97.3% 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 2.25 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