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 4.6 g of methyl trifluoroacetate 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, trimethoxysilylpropyldimethylamine and methyl trifluoroacetate 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 trifluoroacetate.

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. customtrimethoxysilylpropyldimethylamine and methyl trifluoroacetate 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