2-Hydrazinopyrazine → methyl[3-methyl-5-phenyl-1-(pyrazin-2-yl)-1H-pyrazol-4-yl]acetate

HRID 2068478노트

반응식

HRID 2068478 반응식
[NH:1]([C:3]1[CH:4]=[N:5][CH:6]=[CH:7][N:8]=1)[NH2:2].O=[C:10]([CH3:25])[CH:11]([C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=O)[CH2:12][C:13]([O:15][CH3:16])=[O:14]>C(O)C>[CH3:16][O:15][C:13](=[O:14])[CH2:12][C:11]1[C:10]([CH3:25])=[N:2][N:1]([C:3]2[CH:4]=[N:5][CH:6]=[CH:7][N:8]=2)[C:17]=1[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

참가 물질

4

반응물 2

HCID 14878232-HydrazinopyrazineHCID 10657319Methyl 3-benzoyl-4-oxopentanoate

생성물 1

HCID 131730041methyl[3-methyl-5-phenyl-1-(pyrazin-2-yl)-1H-pyrazol-4-yl]acetate

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
135 °C

실험 절차

0.378 g (3.330 mmol) of 3-hydrazinopyrazine in 12.5 ml of ethanol was added to 0.600 g (2.561 mmol) of methyl 4-oxo-3-(phenylcarbonyl)pentanoate, and the mixture was heated at 135° C. in a sealed vessel in a microwave oven for 1.5 h. The solvent was removed under reduced pressure, and the residue was taken up in dichloromethane and washed twice with in each case 25 ml of water. The combined organic phases were dried over sodium sulfate and the solvent was removed under reduced pressure. Chromatography of the residue gave 0.115 g (13.8% of theory) of a light-yellow wax.

후처리

  1. customThe solvent was removed under reduced pressure
  2. washwashed twice with in each case 25 ml of water
  3. dry with materialThe combined organic phases were dried over sodium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customChromatography of the residue gave 0.115 g (13.8% of theory) of a light-yellow wax

출처 및 근거

ORD 기록
ord-c65a45ca98364aad901fab237359ab2e
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08298994B2

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