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Methanol → 3-Nitropropiophenone thiosemicarbazone

HRID 1921592
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HRID 1921592 반응식
[N+:1]([CH2:4][CH2:5][C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=O)([O-:3])=[O:2].CO.[NH2:16][NH:17][C:18]([NH2:20])=[S:19]>CC(O)=O>[N+:1]([CH2:4][CH2:5][C:6](=[N:16][NH:17][C:18]([NH2:20])=[S:19])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([O-:3])=[O:2]
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참가 물질

5

반응물 3

HCID 887MethanolHCID 5694913-Nitro-1-phenylpropan-1-oneHCID 2723789Thiosemicarbazide

생성물 1

HCID 866288283-Nitropropiophenone thiosemicarbazone수율 60.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Into a round bottom flask containing 3-nitropropiophenone (1.02 g, 5.53 mmol), 30 mL of anhydrous methanol were added and the solution was refluxed for about 15 minutes. To the warm ketone solution, thiosemicarbazide (0.485 g, 5.33 mmol) and 1% solution of HOAc (0.4 mL) were added. The reaction mixture was refluxed under nitrogen atmosphere for 30 h, at which point, the solvent was evaporated and, the crude reaction mixture was purified by flash chromatography (50% EtOAc/50% hex) to obtain 0.8119 g (3.22 mmol) of the product in a 58% yield.

후처리

  1. additionwere added
  2. temperaturethe solution was refluxed for about 15 minutes
  3. temperatureThe reaction mixture was refluxed under nitrogen atmosphere for 30 h, at which point
  4. customthe solvent was evaporated
  5. customthe crude reaction mixture
  6. customwas purified by flash chromatography (50% EtOAc/50% hex)

출처 및 근거

ORD 기록
ord-157b7d9d87534e4b93beba76647476b8
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08173696B2

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