2-(Dimethylamino)ethanol → 2-(N,N-dimethylamino)-ethyl 1-pyrrolidineacetate
Reaktionsgleichung
[N:1]1([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].[CH3:14][N:15](CCO)[CH3:16]>>[N:1]1([CH2:6][C:7]([O:9][CH2:10][CH2:11][N:15]([CH3:16])[CH3:14])=[O:8])[CH2:5][CH2:4][CH2:3][CH2:2]1Komponenten
4
Reaktionsbedingungen
- Temperatur
- 150 °C
Versuchsvorschrift
To a mixture of 80 g (0.51 mol) of ethyl 1-pyrrolidineacetate and 0.5 g of sodium hydride (in the form of a 60% by weight suspension in mineral oil) was added 48 g (0.54 mol) of 2-(N,N-dimethylamino)ethanol. The mixture was purged with nitrogen gas, heated gradually and then maintained at about 150° C. while collecting the ethanol by-product in a Dean-Stark trap. The liquid reaction product was distilled at 85° C. at a pressure of 100 μmHg to provide 2-(N,N-dimethylamino)-ethyl 1-pyrrolidineacetate. The structure of the product was confirmed by nuclear magnetic resonance and infrared spectral analysis.