반응 #5605

ord-f0f08fb4c13d448a91c7baff3cb35ade

반응 조건

온도
150°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05244997uspto-grants-1993_09