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Triethylamine → 1-{[(3-Nitropyridin-2-yl)amino]methyl}-4-propylpyrrolidin-2-one

HRID 1896381
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HRID 1896381 반응식
[NH2:1][CH2:2][N:3]1[CH2:7][CH:6]([CH2:8][CH2:9][CH3:10])[CH2:5][C:4]1=[O:11].Cl[C:13]1[C:18]([N+:19]([O-:21])=[O:20])=[CH:17][CH:16]=[CH:15][N:14]=1.C(N(CC)CC)C>O1CCOCC1>[N+:19]([C:18]1[C:13]([NH:1][CH2:2][N:3]2[CH2:7][CH:6]([CH2:8][CH2:9][CH3:10])[CH2:5][C:4]2=[O:11])=[N:14][CH:15]=[CH:16][CH:17]=1)([O-:21])=[O:20]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 796132-Chloro-3-nitropyridineHCID 536292181-(Aminomethyl)-4-propylpyrrolidin-2-one

생성물 1

HCID 577430171-{[(3-Nitropyridin-2-yl)amino]methyl}-4-propylpyrrolidin-2-one수율 53%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 1-(aminomethyl)-4-propylpyrrolidin-2-one x76 (1 eq, 17.09 mmol, 2.67 g), 2-chloro-3-nitropyridine (1 eq, 17.09 mmol, 2.709 g) and triethylamine (1.1 eq, 18.8 mmol, 1.902 g, 2.62 ml) in dioxane (20 ml) is refluxed 48 h. After cooling, the crude mixture is filtrated and the dioxane is distilled under vacuum. The residue is purified by preparative chromatography to afford 2.5 g of 1-{[(3-nitropyridin-2-yl)amino]methyl}-4-propylpyrrolidin-2-one x77.

후처리

  1. temperatureis refluxed 48 h
  2. temperatureAfter cooling
  3. filtrationthe crude mixture is filtrated
  4. distillationthe dioxane is distilled under vacuum
  5. customThe residue is purified by preparative chromatography

출처 및 근거

ORD 기록
ord-d43b31158b7f4b6a851278066e337bd5
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08518943B2

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