2-(Dimethylamino)ethanol → 2-(N,N-dimethylamino)-ethyl 1-pyrrolidineacetate

HRID 5509

반응식

HRID 5509 반응식
[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]1

참가 물질

4

반응물 3

HCID 79022-(Dimethylamino)ethanolHCID 24758Sodium hydrideHCID 2109961-Pyrrolidineacetic acid, ethyl ester

생성물 1

HCID 543299652-(N,N-dimethylamino)-ethyl 1-pyrrolidineacetate

반응 조건

온도
150 °C

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.

후처리

  1. customThe mixture was purged with nitrogen gas
  2. temperatureheated gradually
  3. customwhile collecting the ethanol by-product in a Dean-Stark trap
  4. customThe liquid reaction product
  5. distillationwas distilled at 85° C. at a pressure of 100 μmHg

출처 및 근거

ORD 기록
ord-f0f08fb4c13d448a91c7baff3cb35ade
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05244997

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