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Water → 3-(3-but-3-enyl-2-oxo-pyrrolidin-1-yl)-N-[3-chloro-1-(3-pyridyl)pyrazol-4-yl]-N-ethyl-propanamide

HRID 929320
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HRID 929320 반응식
[CH2:1]([CH:5]1[CH2:9][CH2:8][NH:7][C:6]1=[O:10])[CH2:2][CH:3]=[CH2:4].[H-].[Na+].[Cl:13][C:14]1[C:18]([N:19]([CH2:25][CH3:26])[C:20](=[O:24])[CH2:21][CH2:22]I)=[CH:17][N:16]([C:27]2[CH:28]=[N:29][CH:30]=[CH:31][CH:32]=2)[N:15]=1.O>CN(C=O)C>[CH2:1]([CH:5]1[CH2:9][CH2:8][N:7]([CH2:22][CH2:21][C:20]([N:19]([C:18]2[C:14]([Cl:13])=[N:15][N:16]([C:27]3[CH:28]=[N:29][CH:30]=[CH:31][CH:32]=3)[CH:17]=2)[CH2:25][CH3:26])=[O:24])[C:6]1=[O:10])[CH2:2][CH:3]=[CH2:4]
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참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 149746223-(3-Buten-1-YL)-2-pyrrolidinoneHCID 118023001HCID 118023001, 화합물

생성물 1

HCID 1180234813-(3-but-3-enyl-2-oxo-pyrrolidin-1-yl)-N-[3-chloro-1-(3-pyridyl)pyrazol-4-yl]-N-ethyl-propanamide

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
2회

실험 절차

To 3-chloro-N-(3-chloro-1-(pyridin-3-yl)-1H-pyrazol-4-yl)-N-ethylpropan amide (0.500 g, 1.60 mmol) in acetone (8 mL) was added sodium iodide (0.359 g, 2.40 mmol). The reaction was heated to reflux for 24 hours. The reaction product was filtered and concentrated to provide N-(3-chloro-1-(pyridin-3-yl)-1H-pyrazol-4-yl)-N-ethyl-3-iodopropanamide (0.363 g, 0.898 mmol), which was used immediately without further purification. To 3-(but-3-en-1-yl)pyrrolidin-2-one (0.125 g, 0.898 mmol) dissolved in DMF (4.49 ml) was added sodium hydride (60% in mineral oil, 0.0360 g, 0.898 mmol). The reaction stirred for 45 minutes. Then, N-(3-Chloro-1-(pyridin-3-yl)-1H-pyrazol-4-yl)-N-ethyl-3-iodopropanamide (0.363 g, 0.898 mmol) was added as a solution in DMF (2 mL). The reaction mixture was allowed to stir at room temperature overnight. The reaction product was poured into water, extracted with diethyl ether, and washed with brine. The organics were dried and concentrated to give an oil that was purified by flash column chromatography using 0-60% acetone/hexanes as eluent providing the title compound as a clear, colorless oil. (0.257 g, 69%).

후처리

  1. customwas used immediately without further purification
  2. stirringto stir at room temperature overnight
  3. extractionextracted with diethyl ether
  4. washwashed with brine
  5. customThe organics were dried
  6. concentrationconcentrated
  7. customto give an oil that
  8. customwas purified by flash column chromatography

출처 및 근거

ORD 기록
ord-34f99688bdc6451f866432753aee1315
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09295260B2

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