反应详情

温度

80 °C

A 1-liter separable flask equipped with a nitrogen gas inlet, thermometer, Dimroth condenser and dropping funnel was charged with 310.0 g (2.0 mol) of 1,6-dichlorohexane and heated at 80° C. With stirring, the reaction product of 3-mercaptopropyltriethoxysilane with sodium ethylate was slowly added dropwise. After the completion of dropwise addition, the solution was continuously stirred at 80° C. for 5 hours, and then cooled. From the solution, the salt was filtered off and the ethanol and excess 1,6-dichlorohexane were distilled off in vacuum. The residual solution was subjected to vacuum distillation, collecting 64.2 g of a colorless clear liquid at a boiling point of 148–150° C./0.005 Torr. On analysis by IR, 1H-NMR and MS, the liquid was identified to be a compound of the following formula. (CH3CH2O)3Si(CH2)3S(CH2)6Cl Analysis by gas chromatography gave a purity of 98.7%.

1. customA 1-liter separable flask equipped with a nitrogen gas inlet
2. additionAfter the completion of dropwise addition
3. stirringthe solution was continuously stirred at 80° C. for 5 hours
4. temperaturecooled
5. filtrationFrom the solution, the salt was filtered off
6. distillationthe ethanol and excess 1,6-dichlorohexane were distilled off in vacuum
7. distillationThe residual solution was subjected to vacuum distillation
8. customcollecting 64.2 g of a colorless clear liquid at a boiling point of 148–150° C./0.005 Torr