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

HRID 1718801
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HRID 1718801 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매
HCID 962
Water
용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-fc1f42ac2cce49808c656e8196158f90
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07803940B2

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