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Dimethylcarbamoyl Chloride → 1-((3-chloro-1-(pyridin-3-yl)-1H-pyrazol-4-yl)(ethyl)amino)-1-oxopropan-2-yl dimethylcarbamate

HRID 929306
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HRID 929306 반응식
[Cl:1][C:2]1[C:6]([N:7]([CH2:13][CH3:14])[C:8](=[O:12])[CH:9]([OH:11])[CH3:10])=[CH:5][N:4]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)[N:3]=1.[CH3:21][N:22]([CH3:26])[C:23](Cl)=[O:24]>C(Cl)Cl>[CH3:21][N:22]([CH3:26])[C:23](=[O:24])[O:11][CH:9]([CH3:10])[C:8]([N:7]([C:6]1[C:2]([Cl:1])=[N:3][N:4]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)[CH:5]=1)[CH2:13][CH3:14])=[O:12]
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참가 물질

4

반응물 2

HCID 6598Dimethylcarbamoyl ChlorideHCID 86700598N-(3-chloro-1-(pyridin-3-yl)-1H-pyrazol-4-yl)-N-ethyl-2-hydroxypropanamide

생성물 1

HCID 1180239331-((3-chloro-1-(pyridin-3-yl)-1H-pyrazol-4-yl)(ethyl)amino)-1-oxopropan-2-yl dimethylcarbamate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirred solution of N-(3-chloro-1-(pyridin-3-yl)-1H-pyrazol-4-yl)-N-ethyl-2-hydroxypropanamide (0.10 g, 0.34 mmol) in CH2Cl2 (1.1 mL) was added dimethylcarbamic chloride (0.073 g, 0.68 mmol). The reaction mixture was stirred at room temperature for 16 hours, and then diluted with CH2Cl2, washed with water. The phases were separated, dried and concentrated. The residue was purified by basic alumina gel chromatography eluting with 0%-70% acetone/hexanes to afford the title compound F93 as a light yellow oil (0.11 g, 87%).

후처리

  1. washwashed with water
  2. customThe phases were separated
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by basic alumina gel chromatography
  6. washeluting with 0%-70% acetone/hexanes

출처 및 근거

ORD 기록
ord-d8b0aa2acb7d496db740ba7a700c3e45
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09295260B2

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