反应详情

5.0 g of trimethoxysilylpropyldimethylamine and 18 g of ethyl acetate were charged into a 100 mL flask to be dissolved. While stirring the resultant mixed solution with a magnetic stirrer, to the mixed solution, a solution in which 5.9 g of methyl trifluoromethanesulfonate was dissolved in 24 g of ethyl acetate was gradually added at room temperature in a nitrogen atmosphere. The reaction mixture was refluxed over 3 days and therefrom, ethyl acetate was distilled off under reduced pressure. The resultant concentrate was dropped into 100 mL of diethyl ether and therefrom, trimethoxysilylpropyldimethyl amine and methyl trifluoromethanesulfonate as by-products were removed. This purification was repeated three times and then remaining diethyl ether was distilled off under reduced pressure, followed by dissolving the resultant concentrate in methanol to obtain a 30% methanol solution of trimethoxysilylpropyltrimethylammonium trifluoromethanesulfonate.

1. dissolutionto be dissolved
2. additionmixed solution with a magnetic stirrer
3. additionwas gradually added at room temperature in a nitrogen atmosphere
4. temperatureThe reaction mixture was refluxed over 3 days
5. distillationethyl acetate was distilled off under reduced pressure
6. concentrationThe resultant concentrate
7. additionwas dropped into 100 mL of diethyl ether
8. customtrimethoxysilylpropyldimethyl amine and methyl trifluoromethanesulfonate as by-products were removed
9. customThis purification
10. distillationremaining diethyl ether was distilled off under reduced pressure
11. dissolutionby dissolving the resultant
12. concentrationconcentrate in methanol