Reaktion #5605

ord-f0f08fb4c13d448a91c7baff3cb35ade

Reaktionsgleichung

CCOC(=O)CN1CCCC1
ethyl 1-pyrrolidineacetate
[H-].[Na+]
sodium hydride
CN(C)CCO
2-(N,N-dimethylamino)ethanol
CN(C)CCOC(=O)CN1CCCC1
2-(N,N-dimethylamino)-ethyl 1-pyrrolidineacetate

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture was purged with nitrogen gas
  2. 2
    Temperaturheated gradually
  3. 3
    Sonstigewhile collecting the ethanol by-product in a Dean-Stark trap
  4. 4
    SonstigeThe liquid reaction product
  5. 5
    workup.DISTILLATIONwas distilled at 85° C. at a pressure of 100 μmHg

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05244997uspto-grants-1993_09