Ethyl Acetate → 2-butyl-5-(3,3-dimethyl-2-oxobutyl)-6-methylpyrimidin-4(3H)-one

HRID 1674127노트

반응식

HRID 1674127 반응식
[C:1]([CH:4]([CH2:10][C:11](=[O:16])[C:12]([CH3:15])([CH3:14])[CH3:13])[C:5]([O:7]CC)=O)(=O)[CH3:2].[C:17](=[NH:23])([NH2:22])[CH2:18][CH2:19][CH2:20][CH3:21].C[O-].[Na+].CO.C(OCC)(=O)C>CO.O>[CH2:18]([C:17]1[NH:23][C:5](=[O:7])[C:4]([CH2:10][C:11](=[O:16])[C:12]([CH3:13])([CH3:14])[CH3:15])=[C:1]([CH3:2])[N:22]=1)[CH2:19][CH2:20][CH3:21]

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 4097830PentanimidamideHCID 11775940Ethyl 2-acetyl-5,5-dimethyl-4-oxohexanoateHCID 23694274Sodium methanolate methanol

생성물 1

HCID 1361467962-butyl-5-(3,3-dimethyl-2-oxobutyl)-6-methylpyrimidin-4(3H)-one

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of ethyl 2-acetyl-5,5-dimethyl-4-oxohexanoate (1.04 g) and pentanimidamide (0.89 g) in methanol (10 mL) was added 28% sodium methoxide-methanol solution (3.7 mL), 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 (0.34 g, 36%).

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-ae65ecd186a84f9995ac4e48b4039047
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998968B2

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