反应详情

In a second reaction step, (EtO)3Si—CH2CH2CH2—NH—CO—NH—CH2CH2—Cl (100.00 g, 0.31 mol, 2.00 eq) is initially charged in ethanol (75 ml) in a 500 ml three-neck flask with stirrer, reflux condenser and internal thermometer. Dry sodium sulphide (Na2S, 14.47 g, 0.18 mol, 1.17 eq) is added 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 (93.34 g, 99.2% of theory) is obtained as a waxy, light green solid.

1. temperaturereflux condenser
2. temperaturethe mixture is heated to reflux
3. filtrationthe suspension is filtered
4. customThe filtrate is freed of the solvent on a rotary evaporator
5. customdried under reduced pressure