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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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5-amino-3H-pyrazol-3-one → 7-(2,3-Dichlorophenyl)-1,2,4,7-tetrahydro-5-methyl-2-oxopyrazolo[1,5-a]pyrimidine-6-carboxylic acid, ethyl ester

HRID 1252989
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HRID 1252989 반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]=[C:10]([C:16](=O)[CH3:17])[C:11]([O:13][CH2:14][CH3:15])=[O:12].[NH2:19][C:20]1[N:21]=[N:22][C:23](=[O:25])[CH:24]=1>CN(C)C=O.C(OCC)(=O)C>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]1[N:21]2[NH:22][C:23](=[O:25])[CH:24]=[C:20]2[NH:19][C:16]([CH3:17])=[C:10]1[C:11]([O:13][CH2:14][CH3:15])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 42555565-amino-3H-pyrazol-3-oneHCID 54112468Ethyl 2-[(2,3-dichlorophenyl)methylidene]-3-oxobutanoate

생성물 1

HCID 141304317-(2,3-Dichlorophenyl)-1,2,4,7-tetrahydro-5-methyl-2-oxopyrazolo[1,5-a]pyrimidine-6-carboxylic acid, ethyl ester수율 38.6%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate
용매

실험 절차

A solution of 2-[(2,3-dichlorophenyl)methylene]-3-oxobutanoic acid, ethyl ester (2.8 g; 10.0 mmole) in dimethylformamide (7 ml) was treated with 3-amino-5-pyrazolone (990 mg) and the resulting mixture was heated at 65° C.±5° for 15 hours. The reaction mixture was allowed to cool to room temperature and then diluted with ethyl acetate. The solution was washed with water, brine, and dried over anhydrous magnesium sulfate. Evaporation of the solvent provided a foam which was purified by flash chromatography (7% methanol in dichloromethane). The product was crystallized from acetonitrile-isopropyl ether to provide the title compound as a solid (1.42 g; melting point 213°-218° C.; sinters above 155° C.).

후처리

  1. temperaturethe resulting mixture was heated at 65° C.±5° for 15 hours
  2. washThe solution was washed with water, brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customEvaporation of the solvent
  5. customprovided a foam which
  6. customwas purified by flash chromatography (7% methanol in dichloromethane)
  7. customThe product was crystallized from acetonitrile-isopropyl ether

출처 및 근거

ORD 기록
ord-f78e2d7279a34a54a79cf6d7d830d5ac
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04746656

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