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Ethyl benzoylacetate → 2-Methyl-6-phenyl-4-pyrimidinol

HRID 2063598
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HRID 2063598 반응식
[O-]CC.[Na+].CCO[C:8]([CH2:10][C:11]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=O)=[O:9].Cl.[C:20]([NH2:23])(=[NH:22])[CH3:21]>>[CH3:21][C:20]1[NH:23][C:8](=[O:9])[CH:10]=[C:11]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[N:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 7170Ethyl benzoylacetateHCID 67170Acetamidine monohydrochlorideHCID 2723922Sodium ethoxide

생성물 1

HCID 1354430772-Methyl-6-phenyl-4-pyrimidinol수율 21%

실험 절차

To a freshly prepared solution of sodium ethoxide (18 g of sodium metal was dissolved in 1 L of ethanol), was added ethyl benzoyl acetate (75 g, 0.39 mol) and the mixture was stirred at room temperature for 30 min. To this was added acetamidine hydrochloride (37 g, 0.39 mol) in portions and the mixture was refluxed for 24 h under nitrogen. The reaction mixture was cooled and excess ethanol was removed under vacuum. The residue was acidified to pH=4 with 1.5N HCl and the precipitate was filtered and dried under suction to afford 15 g (21%) of the titled compound as a white solid.

후처리

  1. temperaturethe mixture was refluxed for 24 h under nitrogen
  2. temperatureThe reaction mixture was cooled
  3. customexcess ethanol was removed under vacuum
  4. filtrationthe precipitate was filtered
  5. customdried under suction

출처 및 근거

ORD 기록
ord-5ad7c666c69b4af6b928f15cb9173311
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288398B2

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