Reaktion #5606

Reaktionsgleichung

sodium hydride

ethyl 1-pyrrolidineacetate

2-(1-pyrrolidinyl)ethanol

→

2-(1-PYRROLIDINYL)ETHYL 1-PYRROLIDINEACETATE

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe ethanol by-product was collected in a Dean-Stark trap
2. 2
   TemperaturThe reaction mixture was cooled to about 25° C.
3. 3
   workup.ADDITION12 g of 1-bromopropane was added
4. 4
   Sonstigeto react any alkoxide present
5. 5
   SonstigeThe sodium bromide by-product was removed by filtration
6. 6
   workup.DISTILLATIONThe desired product 2-(1-pyrrolidinyl)ethyl 1-pyrrolidineacetate was purified by distillation at 95° C. at a pressure of 250 μmHg

Vorschrift

To a mixture of 1.3 g of sodium hydride (in the form of a 60% by weight suspension in mineral oil) and 100 g (0.64 mol) of ethyl 1-pyrrolidineacetate was added 91 g of 2-(1-pyrrolidinyl)ethanol. The mixture was heated slowly to about 225° C., and the ethanol by-product was collected in a Dean-Stark trap. The reaction mixture was cooled to about 25° C., then 12 g of 1-bromopropane was added to react any alkoxide present. The sodium bromide by-product was removed by filtration. The desired product 2-(1-pyrrolidinyl)ethyl 1-pyrrolidineacetate was purified by distillation at 95° C. at a pressure of 250 μmHg. The structural assignment was confirmed by mass spectral analysis.

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