Triethylamine → 5-amino-1-(2-methylphenyl)-1H-pyrazole-4-carbonitrile
反応式
Cl.[CH3:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][NH2:10].C(O[CH:14]=[C:15]([C:18]#[N:19])[C:16]#[N:17])C.C(N(CC)CC)C>CO>[NH2:19][C:18]1[N:9]([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[CH3:2])[N:10]=[CH:14][C:15]=1[C:16]#[N:17]参加物
5
実験手順
10.2 g (64.4 mmol) of 2-methylphenylhydrazine hydrochloride are suspended with 7.8 g (64.4 mmol) of ethoxymethylenemalononitrile in 100 ml of methanol, and 26.9 ml (193.3 mmol) of triethylamine are added. The reaction mixture is heated to reflux overnight, during which a clear solution forms. The solution is subsequently distilled off under reduced pressure, and the crude product is purified by column chromatography (silica gel, mobile phase dichloromethane). 10.8 g (85% of theory) of the desired product are obtained.
後処理
- additionare added
- temperatureThe reaction mixture is heated
- temperatureto reflux overnight, during which a clear solution forms
- distillationThe solution is subsequently distilled off under reduced pressure
- customthe crude product is purified by column chromatography (silica gel, mobile phase dichloromethane)
出典と根拠
- ORDレコード
- ord-e92987e2a5984d0a9be6acbba74587cc
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08809348B2
反応ノート
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