反应详情

In 116 g of dehydrated chloroform (reagent, Wako Pure Chemical Ind. Ltd.) was dissolved 24.3 g of N-methoxymethyl-N-methylpyrrolidinium chloride. To the solution was added dropwise 24.3 g of trifluoromethane sulfonic acid (reagent, Aldrich Corp.) at 5° C. over a period of 1 hour. The mixture was reacted at room temperature for 2 hours with gradual increase of temperature. The reaction mixture was concentrated and dried in a vacuum. The residue was purified through alumina column (ICN Biomedicals. GmbH, ICN Alumina N, Act.1/eluent acetonitrile). The eluate was concentrated and dried in a vacuum to obtain 39.1 g of the desired product (colorless liquid).

1. customThe mixture was reacted at room temperature for 2 hours
2. temperaturewith gradual increase of temperature
3. concentrationThe reaction mixture was concentrated
4. customdried in a vacuum
5. customThe residue was purified through alumina column (ICN Biomedicals. GmbH, ICN Alumina N, Act.1/eluent acetonitrile)
6. concentrationThe eluate was concentrated
7. customdried in a vacuum