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

HRID 5509

反応式

HRID 5509 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

反応条件

温度
150 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f0f08fb4c13d448a91c7baff3cb35ade
出典データセット
uspto-grants-1993_09
特許番号
US05244997

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