Ethyl Acetate → 5-benzyl-6-methyl-2-propylpyrimidin-4(3H)-one

HRID 1674131ノート

反応式

HRID 1674131 の反応式
[CH2:1]([CH:8]([C:14](=O)[CH3:15])[C:9]([O:11]CC)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[C:18](=[NH:23])([NH2:22])[CH2:19][CH2:20][CH3:21].C[O-].[Na+].CO.C(OCC)(=O)C>CO.O>[CH2:1]([C:8]1[C:9](=[O:11])[NH:23][C:18]([CH2:19][CH2:20][CH3:21])=[N:22][C:14]=1[CH3:15])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 4

HCID 8857Ethyl AcetateHCID 246929Ethyl alpha-benzylacetoacetateHCID 12828983Butanimidamide hydrochlorideHCID 23694274Sodium methanolate methanol

生成物 1

HCID 1361468715-benzyl-6-methyl-2-propylpyrimidin-4(3H)-one

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of ethyl 2-benzyl-3-oxobutanoate (2.13 mL) and butanimidamide hydrochloride (2.05 g) in methanol (50 mL) was added 28% sodium methoxide-methanol solution (5.8 g), and the mixture was stirred at room temperature for 24 hr. Ethyl acetate and water were added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography to give the title compound as a pale-yellow viscous substance (1.61 g, 66%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated
  5. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-857ca38d3af44becb697aed87c5545df
出典データセット
uspto-grants-2011_08
特許番号
US07998968B2

反応ノート

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