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

HRID 2063598
ノート
印刷プレビュー

反応式

HRID 2063598 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 7170Ethyl benzoylacetateHCID 67170Acetamidine monohydrochlorideHCID 2723922Sodium ethoxide

生成物 1

HCID 1354430772-Methyl-6-phenyl-4-pyrimidinol収率 21%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5ad7c666c69b4af6b928f15cb9173311
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08288398B2

反応ノート

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