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

HRID 2068478ノート

反応式

HRID 2068478 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
135 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c65a45ca98364aad901fab237359ab2e
出典データセット
uspto-grants-2012_10
特許番号
US08298994B2

反応ノート

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